System and method of dosing a polymer mixture with a first solvent, device, system and method of extracting solvent from at least one polymeric yarn, system and method of mechanical pre-recovery of at least one liquid in at least one polymeric yarn, and continuous system and method for producing at least one polymeric yarn

ABSTRACT

The present invention is directed to a method and a system for the production of at least one polymeric yarn comprising means for mixing a polymer ( 1 ) with a first solvent yielding a mixture; means for homogenizing the mixture; means for rendering the mixture inert ( 21, 22, 23 ); means for dipping the mixture into a quenching bath ( 30 ), wherein an air gap is maintained before the mixture reaches the quenching bath ( 30 ) liquid surface forming at least one polymeric yarn; means for drawing ( 41 ) the at least one polymeric yarn at least once; means for washing ( 5 ) the at least one polymeric yarn with a second solvent that is more volatile than the first solvent; means for heating the at least one polymeric yarn ( 6 ); means for drawing at room temperature ( 7 ) the at least one polymeric yarn at least once; and means for heat drawing ( 8 ) the at least one polymeric yarn at least once. 
     The instant invention also concerns a system and method of dosing a polymer mixture with a first solvent into an extruder ( 26 ), a device ( 5 ), a system and a method of solvent extraction from at least one polymeric yarn, and a method and system of mechanical pre-recovery ( 4 ) of at least one liquid in at least one polymeric yarn.

CROSS REFERENCE TO RELATED APPLICATION

This application is a divisional of U.S. application Ser. No.15/032,826, which was filed in the United States Patent and TrademarkOffice on Apr. 28, 2016.

TECHNICAL FIELD

The present invention is related to a method and equipment for producingultra-high performance yarns. More specifically, the present inventiondescribes a continuous method for producing polyolefin yarns havingultra-high tenacity and modulus according to a suspension dosage system,prior oil recovery machines and high efficiency extractors.

DESCRIPTION OF THE STATE OF THE ART

The term high performance yarn is used to classify highly orientedpolymeric materials in the direction of the fibers which materials arecharacterized by having high mechanical strength and high elasticmodulus, especially considering their density.

A steel cable, for example, comprises steel yarns of high tensilestrength, which is around 2 to 3 GPa and an elastic modulus of about 200GPa. A high performance aramid yarn, for example, from the Kevlar®product family (manufactured by DuPont) or Twaron® (manufactured byTeijin), has a tensile strength of between 2.8 and 3.6 GPa and anelastic modulus of between 60 and 70 GPa.

A UHMWPE (ultra-high molecular weight polyethylene) high performanceyarn manufactured by DSM and by Honeywell has a tensile strength ofbetween 3.0 and 3.6 GPa and an elastic modulus of between 80 and 130GPa. However, upon comparing these materials as to their performance incommercial applications, the specific strength, where density is takeninto account, is the most important parameter.

When the material is in the form of a yarn, the specific strengththereof is given by the breaking strength divided by its linear density.In the International System of Units, the linear density of textiles isdesignated by tex (weight, in grams, of 1,000 m of yarn) and thespecific strength unit—cN/dtex—is one of the most used units. Thus,densities of the steel, aramid and UHMWPE yarns are, respectively, of7,860 kg/m³, 1,440 kg/m³ and 970 kg/m³. Based on the densities, theirrespective specific strengths are, therefore, between 3 to 4 cN/dtex forsteel yarns, 19 to 24 cN/dtex for aramid yarns and 31 to 37 cN/dtex forUHMWPE yarns. The specific modules are of about 250 cN/dtex for thesteel yarn, between 400 to 500 cN/dtex the aramid one and between 825and 1340 cN/dtex for the UHMWPE yarn.

Due to its specific strength and modulus, the UHMWPE yarn is deemed tobe the yarn having the greater textile performance existing in themarket and for that reason it has been used in noble applications suchas ballistic protection and anchorage of Offshore oil and gas platformsand more recently as a surgical yarn, sports articles and so on.

The great scientific interest that has motivated the industrialdevelopment of high performance yarns came from studies from the 30'sand 50's. Reports published by Carothers et al. and Mark have shown thehigh potential of the mechanical properties of polymeric materials iftheir chains could be oriented in the same direction.

According to the mentioned document, polymeric chains have extremelyhigh theoretical mechanical properties, so if any method of polymericprocessing was capable of providing orientation to these chains,materials of high mechanical performance could be produced. However,only in the 70's the first methods capable of producing these materialswere developed. Among these methods, we can mention spinning andsolidification of liquid crystals generating the Kevlar®, carbonizationof precursor polymeric fibers giving rise to the carbon fiber,superdrawing of yarns and linear polyethylene films and crystallizationof flexible molecular chains under high elongational flow, whichresulted in a series of materials of high elastic modulus and highmechanical strength.

In this context, in the late 70's G. C. E. Meihuizen, N. A. J. Penningsand G. A. Zwijnenburg published document U.S. Pat. No. 4,137,394, whichdescribes a method for the production of a UHMWPE yarn based on themolecular orientation of the UHMWPE polymeric chains in solution underhigh elongational flow obtained in an equipment based on the Couetteapparatus. However, this production method was still very littleproductive to render the UHMWPE yarn industrially viable.

Publication of document U.S. Pat. No. 4,137,394 has motivated a seriesof important scientific and technological publications, wherein severalmethods for producing this material are proposed. Then in the early80's, there were published patent documents that provided the two mainpreparation processes that currently dominate the International Marketof the UHMWPE yarn. Such yarn is known by the acronyms HPPE (HighPerformance Polyethylene yarn) and HMPE (High Modulus PolyethyleneYarn).

Document GB 2,042,414A discloses a method for the manufacture of highperformance yarns that is currently known as “volatile solvent based gelspinning process” or “decalin based gel spinning process”, hereinaftersimply designated as “decalin based process”. This method was marketedunder the brand name Dyneema®.

In the method described therein, a single solvent is used such that anysolvent having a solubility parameter compatible with the polyethyleneand that can stand the thermal conditions of the method can be chosen.However, for practical applications, the decalin solvent became the mostviable technical-economical solution. The main economic advantage ofthis method is that the solvent used to dissolve UHMWPE is evaporated indrawing steps which follow the spinning step, and the heat required fordrawing is also used to evaporate the solvent, which renders thedecalin-based method more attractive when OPEX (operational expenditure)is taken into account.

However, there are several negative aspects related to decalin-basedtechnology that should be taken into account. Because decalin solvent ishighly flammable and potentially explosive, industrial security issuesare highlighted. Thus, isolation of the productive units is required, sothe area where all the electric components are installed must beexplosion-proof.

Therefore, to seek internal inertization of the production units, aconsiderable amount of nitrogen is consumed and/or other securitymeasures are taken, which considerably affect the CAPEX (capitalexpenditures) of production plant facility.

Furthermore, in addition to the industrial safety and capitalexpenditures aspects, another issue that has to be taken into account issalubrity and the environmental impact of using solvents from thedecalin family, which are highly toxic and potentially carcinogenic.This implies in the need for controlling and monitoring the industrialenvironment such that exposure limits are not exceeded. Leaks of thissolvent to the environment can have catastrophic consequences,especially in the aquatic environment.

Document U.S. Pat. No. 4,413,110 discloses a method for the manufactureof high performance yarns that is currently known as “non-volatilesolvent based gel spinning process” or “mineral oil based gel spinningprocess”, hereinafter simply designated as “mineral oil-based process”.This method was marketed under the brand name Spectra®. In spite of thepatent documents describe several solvents, there are significantdifferences between the two methods.

In this method for producing the HMPE yarn, in turn, two solvents areused. The first solvent has the feature of having low vapor pressure(not being significantly volatile under the dissolution and spinningconditions) and having a solubility parameter compatible with UHMWPE.Thus, in contrast to decalin, the solvent does not evaporate duringdrawing in stages before spinning, which causes the use of a second,more volatile solvent to replace it in a step commonly known as washingor extraction step to be required. Any high vapor pressure volatilesolvent may be utilized, as long as it has the ability to dissolve thefirst solvent. Also, due to technical-economic reasons, solvents such asmineral oil are commonly used as the first solvent, as well as n-hexane.

As compared to the decalin-based method, the mineral oil based methodhas the advantage of being cheaper and not dangerous in steps wheremineral oil is present. From the industrial area point of view, thehighest risk steps would be restricted to the yarn washing and dryingunits, where the second solvent is flammable, which reflects in a lowercapital expenditure (CAPEX) in the industrial plant as compared to theexpenditure required for a plant using decalin-based technology.

The main disadvantages of the mineral oil-based method are related tothe need of using a second solvent and a washing or extraction step.While the first solvent is easily removed by evaporation, during thedrawing step of the decalin-based method, mineral oil is very difficultto be extracted. Extraction of mineral oil by n-hexane, for instance, ismade by a difficult dilution mechanism that takes place competitivelywithin the micelles or pores formed during yarn coagulation that occursjust after spinning inside quenching tanks. Chemically, oil,polyethylene and n-hexane are very similar to each other, which makesthe extraction method even harder.

An additional drawback of this method when compared with the decalinmethod is related to the separation or recovery step of both solvents.While separation of oil and n-hexane is an easy method due to the largedifference between the boiling points of the two solvents, purificationof mineral oil is extremely complex.

Oil purification is the removal of n-hexane residues from oil until safelevels are achieved. A small amount n-hexane residue in mineral oil issufficient to reduce the flash point of the oil to undesired levels.Therefore, the larger the volume of mechanically recovered oil prior tothe extraction step, the more economically advantageous the methodbecomes.

As discussed above, another disadvantage of the mineral oil based-methodis related to the difficulty in controlling heterogeneous deformationsthat may take place in the steps of extraction and drying of the yarn.Both the extraction efficiency and the control of heterogeneousdeformations along the yarn are functions of the design of the equipmentused in the extraction and drying units. Every local deformationoccurring heterogeneously in these steps will hardly corrected in thefollowing steps, which significantly reduces the mechanical properties.

Mineral oil recovery and treatment methods used in the currenttechnologies address these aspects in many ways. The greaterrepresentative of this technology, which developed it in the 80's, isHoneywell (Spectra yarn manufacturer). Document U.S. Pat. No. 4,413,110,for example, describes a mineral oil-based method where a yarn isobtained continuously. On page 9 of said document, aspects related toswelling and shrinkage phenomena inside the oil extraction equipment arereported. In document U.S. Pat. No. 4,551,296 a series of secondsolvents (extraction solvents) is tested and the choice for CFCs familysolvents is explained.

Currently, Honeywell is the world's only known manufacturer that usesmineral oil based technology in a continuous manner. Details about theirextraction equipment are not discussed in their patent documents.However, the main disadvantage of the process is related toenvironmental aspects due to using solvents from the chlorofluorocarbonfamily. Using these solvents reduces the industrial risk during theextraction step, as they are not flammable. They have low boiling pointand are not chemically similar to mineral oil, which makes theseparation thereof in the solvent recovery unit easier. Patent documentU.S. Pat. No. 4,551,296 also shows advantages related to the mechanicalproperty level. Such phenomenon could be related to the residual oilgenerated by an ineffective extraction in experiments using n-hexane.

Alternately, due to the high costs involved in the processing of highamounts of oil and water, which are dragged by the yarn into theextractors, some Chinese manufacturers were lead to split the mineraloil-based method into non-continuous steps, which method is commonlyknown as batch method.

Even though the use of this method has certain economic advantages,aspects related to quality control of the yarn, high labor load andenvironmental impact due to the high rate of solvent evaporation inextraction tanks are shown as strong disadvantages of using decantationas a mechanical tool to pre-recover an oil fraction before processing ofthe yarn in the extractor.

Also, quality of the yarns produced by the mineral oil based technologyis related to deformation control (shrinkage and/or drawing) and oilcontent along the yarn. Gel yarn is very sensitive to deformation andoil exudation is directly related to the time and degree of freedom ofthe yarn due to shrinkage. Thus, yarns are deposited on regions of thesettling box where yarn segments are more free to shrink and exude moreoil, which causes uneven deformations along the yarn that are difficultto be corrected in the final (drawing) step.

Additionally, it is difficult to prevent deformation fluctuations in thesteps of feeding the extractors, which can result in a drastic reductionin the mechanical properties of the produced yarns. In order to preventthese deformations, the manufacturer has to reduce the drawing ratio inthe final drawing step, which drastically affects mechanical propertiessuch as tenacity, modulus and creep.

Using tanks for washing the yarn, in turn, has an intrinsic disadvantagerelated to two main aspects. The first is directed to the ratio of thecross-sectional area of the yarn to the cross-sectional area of thetank. In other words, geometric aspects related to the tank cause theuse of a large volume of extraction liquid to be required. Only thoseliquid layers close to the yarn participate in the extraction method. Itcauses a higher liquid feed rate and a higher liquid inventory whichrepresents larger industrial hazard. The second aspect is related to thedifficulty in causing turbulence inside the extraction compartments,wherein turbulence (expressed in Reynolds number) and temperature arethe two driving forces that can be used to increase efficiency of theextractors.

Some modifications are currently being used to improve efficiency of thetanks. However, aspects such as labor costs, high length of the tanks,cost of the tanks and non-availability of continuous pre-recoveryequipment are some factors that cause the Chinese manufacturers to usebatch methods whenever mineral oil based technology is used.

OBJECTS OF THE INVENTION

The object of the present invention is to provide a continuous mineraloil based method for the manufacture of a polyolefin UHMWPE yarn havinga reduced amount of a second solvent.

The present invention is also intended to provide a device forextracting a first solvent used in a method for the manufacture of aUHMWPE yarn having optimized yarn residence time.

Finally, the present invention is intended to provide a suspensiondosing device used to deliver a homogeneous mixture to an extruder in amethod for manufacturing a polyolefin yarn.

BRIEF DESCRIPTION OF THE INVENTION

The present invention is directed to a method and a system for themanufacture of at least one polymeric yarn comprising means for mixing apolymer with a first solvent yielding a mixture; means for homogenizingthe mixture; means for rendering the mixture inert; means for dippingthe mixture into a quenching bath, wherein an air gap is maintainedbefore the mixture reaches the quenching bath liquid surface forming atleast one polymeric yarn; means for drawing the at least one polymericyarn at least once; means for washing the at least one polymeric yarnwith a second solvent that is more volatile than the first solvent;means for heating the at least one polymeric yarn; means for drawing atroom temperature the at least one polymeric yarn at least once; andmeans for heat drawing the at least one polymeric yarn at least once.

The subject invention also concerns a system and method of dosing apolymer mixture with a first solvent into an extruder (26), a device, asystem and a method of solvent extraction from at least one polymericyarn, and a method and system of mechanical pre-recovery of at least oneliquid in at least one polymeric yarn.

DESCRIPTION OF THE FIGURES

The following detailed description makes reference to the accompanyingdrawings, in which:

FIG. 1 illustrates a schematic view of a system for the manufacture ofpolymeric yarns, according to an optional configuration of the presentinvention;

FIG. 2 illustrates a schematic view of a dosing system of a solventmixture with a polymer in accordance with an optional configuration ofthe present invention;

FIG. 3 illustrates a view of a mechanical pre-recovery system of a firstsolvent in accordance with an optional configuration of the presentinvention;

FIG. 4 illustrates a front view and a side view of a washing device fora polymeric yarn in accordance with an optional configuration of thepresent invention;

FIG. 5 illustrates an isolated view of a rotating member and anauxiliary member of the extraction device of FIG. 4;

FIG. 6 illustrates an schematic configuration of a circuitry optionallycomprised in the extractor device of FIG. 4; and

FIG. 7 discloses a diagram showing the yarn and solvent flows and achart illustrating the volumetric compositions of both solvents overtime.

DETAILED DESCRIPTION OF THE INVENTION

The following description will be based on a preferred embodiment of theinvention. As will be evident to the skilled person, however, theinvention is not restricted to this particular embodiment.

According to a preferred embodiment that will be described herein, thepresent invention provides a method for the production of a ultra-highperformance yarn, preferably, a yarn comprising ultra-high molecularweight polyolefin, wherein such yarn is produced with a technology knownas mineral oil based technology.

FIG. 1 illustrates a system for the manufacture of a polyolefin yarncomprising all the units required for the execution of the steps of thepresented optional configuration of the method of the present invention,namely:

(a) mixing, with the aid of the premix vessel 1, the ultra-highmolecular weight polyolefin polymer with the first solvent andadditives;(b) transferring the mixture to a homogenization and inertizationdevice, optionally a homogenization/inertization tank 21,22, where themixture will remain for a time sufficient to become homogeneous andvirtually free of oxygen;(c) dosing the mixture, steadily and intermittently, with the aid of adosing device 25 in an extruder 26;(d) dissolving the polymer in the first solvent under an intensivecondition, within the extruder 26, so as to form a homogeneous solution;(e) dosing the solution in a volumetric and precise manner through anorifice die 27, providing the solution with the shape of a yarn;(f) dipping the solution, in the form of a yarn, in a water bath, knownas a quenching bath 30, such that the yarn, before reaching the watersurface, passes through an air gap for the solution to coagulate therebyforming the polymeric yarn 10 (gel yarn);(g) passing said gel yarn through a tower of feeding rolls 40, such thatpart of the water dragged by the yarn from the quenching bath 30 and afraction of the first solvent, exuded from the yarn in the coagulation,are drained by the action of gravity;(h) drawing 41 the gel yarn 10 in a tank 410 containing a liquid medium;(i) passing the drawn gel yarn through a first pre-recovery enclosure42, wherein the first exuded solvent and liquids dragged from thedrawing tank 410 are mechanically retained;(j) passing the yarn through an accumulator 43 such that the residencetime is sufficient for the exudation method to be complete, exposing agreater volume of a first solvent on the surface of the yarn;(l) passing the gel yarn through a second pre-recovery enclosure 44,wherein the residual solvent fraction exuded by the yarn in theaccumulator 43 can be mechanically retained;(m) feeding the gel yarn containing a reduced fraction of the firstsolvent with a second solvent in an extraction unit 5 (FIGS. 1 to 13);(n) passing the gel yarn, containing the second solvent, through a dryer6, wherein the second solvent is substituted with a heated gas, yieldingxerogel yarn 11;(o) drawing the xerogel yarn between at least two roll towers 7 at roomtemperature;(p) heat drawing the yarn in a draw oven 8 yielding the POY (PreOriented Yarn) yarn; and(q) storing the POY yarn in bobbins 91 in the winding unit 90.

Optionally, a high or ultra-high molecular weight polyolefin is used inthe method for the production of a ultra-high performance yarn of thepresent invention. Polyolefins such as high molecular weightpolyethylene or ultra-high molecular weight polyethylene (UHMWPE), suchas high and ultra-high molecular weight polypropylene and anethene-propene copolymer can be used. However, other polymers can beused, such as polyvinyl alcohol, polyesters, polyoxide ethylene. Morepreferably, ultra-high molecular weight polyethylene (UHMWPE) is used.

For use as a first solvent, any solvent that dissolves the abovepolymers under the method conditions described herein, can be used. Morespecifically, any solvent with a solubility parameter consistent withthe used polyolefin and which supports the operating temperature of themethod can be used. Preferably, any solvent with a solubility parameterconsistent with the used polyolefin and which is not considerablyvolatile at the dissolution temperature can be used. Preferably, mineraloil is used when the polyolefin is ultra-high molecular weightpolyethylene. More preferably, the solvent is preferably chosen fromclasses such as aliphatic hydrocarbons, cycloaliphatic hydrocarbons,aromatic hydrocarbons, halogenated hydrocarbons, and mixtures thereof.In another context, the first solvent should have a vapor pressuregreater than 20 kPa or a boiling point greater than 180° C. and thatdissolves the polymer under the process conditions described in theinvention.

In the context of the instant invention, when ultra-high molecularweight polyethylene is used, the molecular weight (Mw) should be greaterthan 500,000, preferably greater than 1,000,000, and more preferablyeven greater than 2.000.000. When such polyolefin is used, it isrecommendable to use a suitable amount of antioxidant. In addition,substitution of air with nitrogen or any other inert gas in thedissolution conditions is preferably adopted.

The polymer concentration is recognized as one of the main methodvariables in the technology related to the context of the presentinvention. Such polymer concentration in the first solvent is linked totechnical and economic aspects of the method. In context of the presentinvention, the concentration choice will be, therefore, a result of thebalance between the intended better mechanical property and the methodcost. In this regard, the mass concentration range of the polymer in thefirst solvent is from 3 to 30%, preferably, from 5 to 20% and, even morepreferably, of from 8 to 15%.

Referring again to FIG. 1, a schematic representation of the optionalconfiguration of the method of the present invention is shown, where anumber of mixing and dosing devices are placed such that the polymermixture, first solvent and additives can be appropriately added to anextruder 26. For ease of nomenclature, the set formed by all the devicesinvolved in the function of providing a homogeneous mixture in theextruder 26 will be hereinafter designated as dosing device 25.

Furthermore, the system of the present invention comprises a premixvessel 1 where suitable amounts of the components are added such that ahomogeneous mixture is obtained. The premix vessel 1 optionallycomprises a mixing impeller 14, a pumping device 15, preferably of thejet mixing type, to cause the mixture to be constantly stirred from thebottom of the premix vessel to the top thereof. Therefore, the mixtureis homogenized during the required time before being pumped to at leastone inertization device 21,22. For ease of nomenclature, theinertization device will also be designated as inertization vesselherein.

Optionally, the at least one inertization vessel 21,22 still provideshomogenization of the mixture in a similar fashion as the premix vessel.However, the inertization vessel 21,22 further comprises an inertizationgas flow used to extract oxygen from the mixture, thereby causing it tobe inert. The oxygen content in the mixture is optionally monitored bysuitable sensors until acceptable levels are achieved.

Optionally, the system of the present invention comprises twoinertization vessels, as illustrated in FIG. 1.

Dosing of the mixture in the extruder can be made by any dosing deviceknown in the state of the art, provided that it can maintain ahomogeneous solids concentration. The dosing device 25 is intended tocontinually feed the extruder 26 with the homogeneous and inertizedmixture provided by the inertization vessel 21,22.

FIG. 2 illustrates a dosing device 25, or doser, in accordance with apreferred configuration of the present invention, where dosing is madesuch that a low level of mixture is always above the screw 261 of theextruder. To that end, the level is adjusted so as to be between anupper limit (above which a column of liquid with no agitation forms agradient of solid settling) and a lower level that prevents the gas fromentering the extruder. Thus, agitation caused by rotation of theextruder screw will ensure homogeneity of the column of mixture. Forthese settings to be implemented, the dosing device 253 may comprise alevel sensor. Thus, where the level of the mixture inside the dosingdevice 25 is below a pre-determined value, an electrical input deviatesa valve to the tube 254, feeding the dosing vessel 25 until an upperlevel signal reverses the valve back to its original position. In orderto prevent contamination by oxygen from air, a flow of inert gas isoptionally maintained within the vessel 25. To that end, the dosingvessel 25 optionally comprises a gas inlet tube 251 and a gas outlettube 252. It should be emphasized that, as noted, any level controldevice known from the state of the art can be used as the dosage form.However, the above device is preferably used.

Further, the present invention provides the optional use of a start andstop vessel 23 when the described system of preparation, homogenization,inertization and dosing of the mixture is used. Such start and stopvessel 23 is only intended to be used in the beginning and in the end ofthe described method, since it is intended to provide a more dilutedmixture of polymers in the start and final steps of the extruder. Thisallows for the extruder to be started at the normal rotation of themethod, without any damages to the equipment being caused by pressurepeaks, which can occur in a start at high rotation. This procedure thusavoids unbalancing of the method caused by a poor dissolution of themixture present in the inertization vessel. High and ultra-highmolecular weight polymers are hard to dissolve and the unbalance of themethod, which occurs mainly while starting and stopping the extruder,results in clumps or poorly dissolved particles which act as a defect tothe formed yarn, thereby reducing its local drawability. The extruderbeing started under optimal conditions, in addition to preventing thiskind of problem, will lead to rapid stabilization conditions, minimizingthe residue volume at the start.

Optionally, the present invention makes use of only two inertizationdevices 21,22,23 wherein one of the inertization devices, in the stepsof start and end of the extruder 25, feeds the extruder 26 with a morediluted polymer mixture, such that this device is thereafter used withthe mixture with standard dilution.

Optionally, the dosing device is an container, or an tube, which simplydrives the mixture from the inertization device to the extruder. Also,in another optional embodiment, the dosing device is integrated to theextruder, or is part of the extruder.

Therefore, in context of the present invention, the suspension dosagesystem in the extruder, comprises:

a) a premix vessel 1, where all the components of the suspension areadded, comprising a mechanical stirrer and a pumping circuitry, thusensuring a better homogenization of the mixture;b) at least one inertization vessel (optionally two vessels) 21,22,comprising a mechanical stirrer 200, a pumping device 201 (optionally ofthe jet mixing type) constantly circulating the bottom mixture to thetop of the vessel 21,22, am inert gas feeding device and a device formeasuring the oxygen content, such that inertization is ensured;c) a dosing device 25 comprising a level control device 253, such thatthe level of the mixture, as defined by the column of suspension liquidabove the level of the extruder screw, can be controlled, wherein thedosing device is fed by at least one inertization vessel, such that avalve installed on the bottom of the inertization vessel controls saidfeeding and releases a certain volume of suspension when a signal of lowlevel in the dosing vessel is received, optionally, the dosing vessel isfed with a constant flow of inert gas which is maintained throughout theproduction;d) a start and stop vessel 23 used in start and stop operations of theproduction line, comprising a mechanical stirrer 200, a pumping device201 (optionally of the jet mixing type), an inert gas feeding device andan instrument for measuring the oxygen content, optionally the start andstop vessel 23 comprises a reduced volume as compared with theinertization vessel 21,22, wherein the start and stop vessel 23 is fedwith a suspension having low polymer concentration, which yields asolution of lower viscosity and for that reason reduces the startpressures of the extruder, allowing it to be turned on at high rotationspeeds.

The mixture or suspension homogenized and inertized by the abovementioned system then feeds an extruder 26. In context of the presentinvention, any type of extruder known in the state of the art can beused, including, but not limited to single-screw, twin-screw andplanetary extruders. Combinations of one or more extruders may be usedas well, whenever an improvement in the cost effectiveness of the methodis desired. However, in the preferred embodiment now described,twin-screw extruders are preferable.

In the extruder 26 the mixture or suspension is transformed into asolution. Dissolution is a difficult process, where process parametersshould be defined for each case and each setting of the extruder used.In a particular configuration, when ultra-high molecular weightpolyethylene is dissolved in mineral oil, the temperature must bebetween 150° C. and 310° C., more preferably, between 180 and 240° C.

The polymer solution in the first solvent, produced by the extruder, isthen fed to a spinning head 27, which comprises a spinning pump and aspinning die. The spinning pump serves to dose the solution to thespinning die in a precise manner, which in turn serves to impart theshape of a yarn to the fluid. The spinning die or spinneret has adefined number of capillaries. In context of the present invention, thenumber of capillaries is not a critical parameter and depends on factorssuch as the production capacity of the extruder, the spinning technologyused, the intended final titer of the yarn, etc. In the capillary of thespinning die, the bulk of polymer will be subjected to a first molecularorientation, which takes place under shear and elongational flow alongthe capillary.

The yarn of the polymer solution dissolved in the first solvent thenpasses through the air gap and immerses into the quenching bath 30,where the solution coagulates, yielding the so-called gel yarn 10. Inthe scope of the present invention, the term air gap is used to definethe space traversed by the yarn of the solution, from the outer surfaceof the spinning die 27 to the liquid surface of the quenching bath 30.The length of the air gap is another variable is critical importance inthe method of the present invention. However, it will depend on thespinning condition used. The spinning condition is determined by fourvariables, basically, the geometry of the capillary, the temperature,flow rate and the use or not of a drawing step after the quenching bath30. Such drawing will be hereinafter designated as draw down.

When a little or no draw down is adopted, the length of the air gap ispreferably of less than 15 mm, more preferably of less than 10 mm, onthe other hand, the minimal length of the adopted air gap is 2 mm,preferably greater than 4 mm.

However, when draw down stretches are applied to the yarn, the adoptedair gap length is greater than 5 mm, preferably greater than 15 mm.

In turn, as already explained, the quenching bath 30 serves to transformthe solution into a gel yarn. The gel yarn is a structure composed of apre-oriented, polymer-containing porous phase that comprises almost theentire volume of liquid comprising the first solvent. Any liquid, inprinciple, can be used as a quenching liquid, provided that it does notaffect the properties of the yarn. When the polymer used us ultra-highmolecular weight polyethylene, water is the preferred solvent. Thetemperature of the quenching bath must be of less than 60° C.,preferably of less than 30° C., more preferably of less than 20° C.

Then, the gel yarn 10 formed in the quenching bath and containing alarge portion of the volume of the first solvent and water dragged fromthe quenching bath is fed to a pre-recovery and draw unit in a liquidmedium. For ease of nomenclature, the pre-recovery and draw unit inliquid medium will be hereinafter simply designated as pre-recuperator.

A pre-recuperator has a first function of mechanically retaining thelargest volume as possible of the first solvent, such that theextractors are not overloaded, which would increase the operational costof the method. Optionally, the pre-recuperator may perform anintermediate draw on the yarn, which can reduce the draw load that willoccur in subsequent steps. The draw limit in this step is determined bythe beginning of damage to the polymeric structure and is determined bythe final mechanical properties. In the scope of the present invention,the relative amount of the first solvent retained by the pre-recuperatorprior to the extraction step is designated pre-recovered amount ofsolvent and is represented by a pre-recovery index. The pre-recoveryindex is described by the percent ratio of the mass or volume of solventtransported by a certain length of the yarn that exits thepre-recuperator and the yarn entering the pre-recuperator.

As already discussed, one disadvantage, if not the greatest, of themineral oil base technology is the need for recovering a large volume ofthe first solvent using a second, more volatile solvent. When, forexample, the first solvent is mineral oil and the second solvent is ofthe n-hexane type, the separation thereof in a distillation column isrelatively easy due to the large difference in the boiling points of themixture components. However, even if the distillation column is veryefficient, the n-hexane content present in the oil of the bottom of thecolumn remains elevated.

A small n-hexane concentration in the mineral oil is sufficient todrastically reduce its flash point, which generates an industrial hazardwhen the oil is recycled to the method. It requires the use of a secondseparation operation herein designated as oil purification. Thepurification step adds up cost to the method since it is a slow and highcost operation. Another issue related to the cost is the volume of thesecond solvent involved in the method. The larger the volume of thefirst solvent entering with the yarn in the extraction unit, thegreatest will be the consumption of the second solvent. Whichconsumption can also be increased by the ineffectiveness of theextractors.

Manipulation of a large volume of the second solvent leads to a greaterinvestment in the solvent recovery unit and higher industrial hazard.One of the criteria for ranking hazard radius is the volume of flammablesolvent present in the industrial area. Another issue related to thevolume of the first solvent is the amount of the second solvent to beevaporated in the drying unit. Since the amount of the first solvent issubstituted with approximately the same amount of the second solvent inthe extraction method, the lower the volume of the first solvententering the extractors, the lower will be the amount of the secondsolvent to be evaporated in the drying unit.

FIG. 3 illustrates an optional configuration of a pre-recovery system 4(or pre-recuperator), in accordance with the present invention,comprising five optional main devices. The first device comprises atower of feeding rolls 40 of the pre-recuperator 4, wherein the numberof rolls 401 depends on factors such as the stretching strength and theminimum contact perimeter for no slippage to occur. In practice, thenumber of rolls 401, as well as the diameter thereof is the result of arelationship between the cost of the machine and the likelihood ofslippage. The number of rolls 401 outlined in FIG. 3 is therefore merelyillustrative.

The tower of feed rolls 40 can also serve as a tower of spinning rolls,that is, to pull yarns formed on the spinning die passing through thequenching bath. Since the yarns passing through the quenching bath carryan amount of water and first solvent, a collector tray can be installedon the lower part of the tower, which will receive any amount of thesesolvents from the rolls.

The pre-recovery system illustrated in FIG. 3 further comprises adrawing tank 410, where a liquid serves to provide heat to the gel yarn,which will be stretched between the feed tower 40 and a firstpre-recovery enclosure 42. The drawing bath basically comprises adrawing tank 401, a lid 412, at least one driver 411 (two drivers areillustrated) for immersion of the yarn into the tank 410, a drain 413, aheat exchanger and a circulation pump.

Using immersion drivers 411 facilitates passing the yarns through thetank 410 during the start operation, such that the drivers 411 arecapable of drawing the yarn inside the tank 410, pushing the yarn to thebottom of the tank 410. The immersion drivers 411 serve, therefore, tomaintain the yarn immersed in the tank 410 after being passed in thestart operation.

The tank 410 can also comprise a lid 412 serving to isolate the systemfrom external contamination, to prevent accidents by the contact of theheated liquid and to thermally isolate the tank.

Circulation of the heated liquid within the tank 410 may be optionallyperformed with the aid of a pump and a heat exchanger, together with aninert gas disperser. Dissolution of the inert gas into the liquid isrecommended when the drawing liquid medium is the mineral oil used asfirst solvent. In a stable stage of the method, an inert gas-containingatmosphere injected into the disperser is formed between the surface ofthe liquid and the lid. The design of the tank must take into account alow inventory and the absence of neutral positions for no additionaldegradation of the first solvent to occur in this step.

The third part of the pre-recuperator comprises a first pre-recoveryenclosure 42. The first pre-recovery enclosure 42 serves to retain themajor portion of the first solvent exuded during drawing in the tank410, as well as the liquid used as a thermal medium in drawing, which isdragged by the yarn. The first pre-recovery enclosure 42 has a rolltower 420 having two main functions, the first is to draw the gel yarnthat passes the drawing bath and the second is of acting as a supportwhere mechanical action of compressed air knives 421 and scrapers 422will retain any liquid contained on the surface of the yarn filaments.

In context of the present invention, compressed air blades 421 areoptionally used to prevent a large portion of the liquid volume draggedby the yarn from passing to the next steps. When yarns containing thefilaments are driven onto the surfaces of rolls 420, the filamentsspread as ribbons. Surprisingly, when compressed air blades 421 are dulydirected tangentially (relative to the roll 420) and transversally(relative to the gel yarn), a major amount of liquid is retained.

Part of the retained liquid is projected away from the roll surface 420and a portion of the liquid is adhered thereto. Therefore, to preventpart of the liquid adhered to the roll 420 from wetting the yarn,optionally a scraper device 422 is designed so as to transfer thisvolume to the end of the roll 420. Devices transforming compressed airinto laminar flows of high speed are found commercially. An example isthe so-called air knives from Spraying Systems Co′ capable ofconcentrating a compressed air jet in very precise geometrical shapes,which considerably reduces air consumption. Optionally, other liquidretention devices can be used, such as rubber-coated devices commonlyknown in the textile industry, such as Foulards.

The use of devices for liquid retention, especially air blades 421, hasshown to be suitable for retaining the mineral oil, wherein one canobserve that air penetrates between the yarn filaments, expelling alarge amount of liquid. The use of air knives, or any device operatingin an obvious manner, along with another support device capable ofremoving the liquid adhered to the surface of the draw roll 420 areconsidered herein as the mechanical driving power that was shown to besufficiently more efficient than decantation and made it possible forone to recover a large volume of the first solvent prior to the use of achemical action (use of the second solvent).

FIG. 3a illustrates in detail an optional embodiment of these devices,where the air knife 421 and the rubber scrapers 422 can be seen over therolls. The representation is schematic and other assembly configurationsare possible. For practical purposes, the above described equipment ismounted inside a housing that encloses it.

Further, a tray 426 is optionally installed on the lower part of theenclosure 42 and serves as a collector of the liquid bulk, while anupper protection 425 serves as a guard to projections of liquid causedby compressed air, such that the upper protection may further comprise atube serving as an obstacle to liquid particles and to the sound, whileletting air pass through.

Drainage of liquid from the bottom of the tray 426 can be made directlyto a solvent recovery area or it can be recycled back to the drawingtank 410 with the aid of a pump. The advantage of the latterconfiguration is that the tank 410 will always have a level that tendsto be greater than the level of a drain. If the liquid accumulated onthe bottom of the tray of the pre-recovery enclosure is directlyconveyed to the solvent recovery area, a liquid feeding device must beinstalled on the drawing tank, ensuring replacement of the liquid mediumlost by dragging of the yarn that is drawn and enters the pre-recoveryenclosure.

Optionally, if one desires to completely isolate the interior of theenclosure 42, a Foulard rubber roll device 423 can be used. Using thesedevices aids in retaining liquid, in addition to isolating theenclosure. However, to ensure that no damages are made to the yarn, alow closure pressure should be used together with low hardness rubbers.

For the purposes of providing hearing comfort, the housing can beoptionally insulated with any sound insulation elements.

In the present context, it is important to define the meaning of freeliquid volume onto the surface of the filament. The gel yarn ischaracterized by a porous structure (very similar to a sponge when seenin cross section) containing a large volume of liquid (first solvent).When the gel yarn is formed, part of the volume of oil is expelled tothe yarn surface. If a segment of gel yarn is let to rest with fixedends, part of the oil will run off on the yarn under the action ofgravity and part of the oil will remain inside the pores in an “stable”manner, being held capillarity forces. Based on this phenomenon, we willdefine hereinafter that the free liquid volume is all the volumetricfraction that can be retained or recovered by a certain mechanicalprinciple.

On the other hand, the stable volumetric fraction is defined as thevolumetric fraction that cannot be recovered by such a mechanicalaction, provided that the mechanical forces involved do not overcome thecapillarity forces. Another important aspect is that liquid exudationcaused by a deformation made while drawing the gel yarn is meant to be aconsequence of the anisotropy given by the orientation. In other words,the crystallization to which the polymer is subjected while being drawn,associated with a change in the aspect ratio of the pores under theaction of the same deformation, is responsible for transforming thestable liquid volume into a free liquid volume. Thus, a major part ofthis phenomenon would take place in the drawing bath.

However, experimental data show that oil exudation by the pores of thegel yarn is a slow method as compared to the average residence time inthe bath and in the first pre-recovery enclosure. In other words, afterdeformation is determined, a certain period of time is required for acorresponding portion of the stable volume to exudate, transforming intothe free portion, such that it can be retained by compressed air blades.In a continuous regimen, this is a problem because while a higher drawratio in the bath allows for a greater displacement of the stableportion to the free portion, the same increase imposes a higher speed ofthe yarn along the internal path of the first pre-recovery enclosure 42,reducing proportionately the residence time for the air blades to beable to work. Such a loss in efficiency with the increase in the drawratio would lead to a proportional increase in the residence time, whichwould increase the cost in equipment.

However, experiments have also shown that withdrawal of the free oil bythe air blades is a fast method as compared with the exudation time. Inother words, to simply increase the path of the yarn in the firstpre-recovery enclosure would not be the most efficient manner to improveretention efficiency, since the cost of the equipment and theconsumption of compressed air would increase considerably.

Therefore, in order to increase efficiency of the pre-recovery unit withthe least impact possible on the cost of the equipment, the idea ofoptionally adopting an accumulator 43 was conceived. In context of thepresent invention, accumulator 43 is any configuration of textileequipment capable of increasing the path of the yarn in the most compactmanner possible, for the time required for the exudation method tooccur.

In the optional configuration disclosed, the accumulator 43 comprisestwo columns of idlers or rolls that can conduct the yarn so as toprevent the occurrence of damages or titer oscillations. Adjustment inthe residence time is carried out by the number of “zig-zag” turns andby the distance. Rolls or idlers can be free or motor-driven.Conceptually, the use of a powered transport system would not berequired, since the two pre-recovery enclosures 42,44 would serve toguide the yarn. However, to prevent that friction variations on the rollor idler axes can cause titer instabilities in the gel yarn, a poweredconfiguration can be optionally adopted. In addition, such a powereddrawing device can be designed such that an elevation gradient can beprovided along the yarn path. This would allow for a small stretch to bemade in the accumulator 43, thereby preventing any degree of relaxationof the gel yarn along the path.

The fifth and last part of the pre-recuperator unit is the secondpre-recovery enclosure 44. The description of the second pre-recoveryenclosure 44 is the same as the first, as described above, such that thesecond enclosure serves to retain the first solvent exuded along thepath of the accumulator.

Conceptually, any liquid may be utilized as a drawing medium in thedrawing tank 410. However, in the scope of the present invention, theliquid itself used as the first solvent or water are preferably adopted.However, any other liquid other than those mentioned above may adverselyaffect the method, since other separation operations must be used, thenburdening the solvent recovery area.

When the liquid itself used as first solvent is used as a thermaltransfer medium in the drawing tank 410, a small pre-recovery enclosure(not shown) can be adapted on the feed tower to retain the water draggedfrom the quenching bath. Experience acquired from experiments using airblades has shown that the water dragged by the wire exiting thequenching bath is relatively easy to retain. Water forms small drops onthe gel yarn surface, being very exposed to the action of air streams.

In practice, the choice of the liquid used in the tank will depend onthe drawing temperature. When the desired work temperature range isbetween room temperature and 80° C., water is the preferred liquid inthe scope of the present invention. The gel yarn has a high amorphousfraction, which enables high draw ratios to be obtained at a temperatureof less than 80° C. On the other hand, the draw ratio is limited by thelow motion of the chains in the crystalline phase. The use oftemperatures of greater than 80° C., achieved by using mineral oil as athermal medium, makes it possible to obtain high draw ratios with nodamage to the microstructure of the gel yarn and, as a result, obtaininghigh pre-recovery index values. In this context, the draw ratio appliedto the gel yarn must be greater than 1.5:1, preferably greater than 5:1and more preferably, greater than 8:1.

While the use of high draw ratios in the gel yarn is beneficial for highfractions of free oil to be obtained, efficiency of pre-recuperators isvery reduced by decreasing the residence time (increased speeds). Tocompensate for that, all the features of the pre-recovery enclosure42,44 must be optimized. The number of sets of air blades 421, 441 mustbe increased at the same proportion as the draw ratio applied to the gelyarn. In context of the present invention, the number of sets of air421, 441 blades must be higher than 1, preferably higher than 4, morepreferably higher than 6. Preferably, the number of sets of air blades421, 441 per roll 420, 440 must be equal to 1. However, a greater numbercan be used. The distance between the air blade 421, 422 and the surfaceof the roll 420, 440 must he adjusted as a function of the compressedair pressure used. Very high pressures associated with small distancesare limited by the entanglement of the yarns and even by thedisplacement of the path thereof on the roll perimeter 420, 440. Incontext of the present invention, the distance between the airblade-generating device 421, 441 and the surface of the roll 420, 440must be lower than 60 mm, preferably lower than 40 mm, more preferablylower than 20 mm. Pressure used in the air blade-generating device 421,441 depends on the device used. However, the used pressure must belimited by the entanglement of the yarn or by another instability thatcan cause any damages to the yarn or any processability problems in thespinline. There are many ways to position the air blade 421, 441relative to the yarn. In context of the present invention, thepreferable positioning is such that flowlines of the air blade 421, 441are directed away from the motion of the yarn and are tangential to theroll surface.

Using textile features to accumulate yarns 43 between the twopre-recovery enclosures 42,44 is the key factor in the efficiency of thepre-recovery unit 4. If a textile configuration is used as shown in FIG.3, the distance and the number of zig-zags must be adjusted such that aresidence time of greater than 0.5 minute is achieved, preferably aresidence time of greater than 1 minute and more preferably greater than2 minutes will be sufficient for the major part of the stable oil to betransformed into free oil.

In context of the present invention, preferably, rolls or idlers used inthe accumulator columns move independently from each other, that is, theuse of powered mechanical devices is preferred. When such aconfiguration is used, the ratio of the speeds of the rolls must beadjusted so as a global draw in the accumulator of greater than 1.05,preferably greater than 1.1 and more preferably greater than 1.2 isapplied. For no damages to occur in the yarn microstructure, a globaldraw ratio in the accumulator must be of less than 5, preferably of lessthan 3 and more preferably of less than 1.5.

Therefore, the pre-recovery system now described optionally comprises:

a) a tower of feed rolls 40 where the number of rolls 401 is sufficientto prevent slippage of the yarns, wherein, optionally, the tower 40 maycontain a liquid retaining device 402 and a first solvent which areoccasionally dragged from the quenching bath 30, and wherein, to preventloss of solvents and water, a collecting tray can be placed below therolls;b) a drawing tank comprising 41 a liquid medium serving to transfer heatto the yarn and to collect the volumetric fraction of the first solventexuded during the residence time in the tank 410, wherein said tank 410contains a system of immersion rolls 411 to facilitate passage of theyarns, wherein the tank can also comprise a liquid circulation pumpcontained in the tank, a heat exchanger, a drain and a lid 412, suchthat, when the liquid used is the first solvent itself, an inert gasfeeding device may be used to prevent degradation of the liquid.c) a first pre-recovery enclosure 42 optionally comprising:

-   -   a second roll tower 420 or a yarn accumulator serving to draw        the gel yarn while it passes through the drawing tank 410, such        that drawing is given by the difference in the speeds between        towers 40,42;    -   air flow generating devices 421, such as air blade devices,        where compressed air is used to retain the volumetric fraction        of the first solvent that is available in the free form, on the        filament surfaces of the yarns, while they are transported by        the rolls of the second tower 42, such that these devices are        preferably directed away from the motion of the yarns and such        that the air blade is tangential to the roll surface;    -   scraper devices 422 duly coupled to the tower rolls 420, serving        to retain liquid adhered to the surface of the rolls 420,        preventing them from wetting the yarns;    -   an external environment-insulating case or housing 425,        comprising walls with some sound-absorbing features, a liquid        collecting tray 426 positioned below the rolls and an air        exhaustion tube installed on the top of the enclosure 42, which        can contain elements that retain liquid and sound particles;        d) a yarn accumulator 43 optionally comprising two roll towers        430 where the yarns can travel a “zig-zag” path in order to        maintain the yarn for a period of time sufficient for the first        solvent to exudate, being available at the surfaces of the yarn        filaments;        e) a second pre-recovery enclosure 44, preferably comprising        features similar to those of the first 42 pre-recovery        enclosure, however, due to a possible increase in the speeds in        the previous steps, the second enclosure may comprise a higher        number of air blade generating devices 441.

Furthermore, according to the optional configuration described herein,the pre-recuperator now proposed optionally comprises:

a) a pre-recovery index expressing the fraction of the first solventretained by the pre-recuperator 44 and which will not contact the secondsolvent in the extraction step, wherein the pre-recovery index isgreater than 20%, preferably greater than 50% and more preferablygreater than 70%;b) drawing in a liquid medium, which takes place between the first tworoll towers of the pre-recuperator, while the yarn is submersed in thetank, characterized by a draw ratio applied to the gel yarn that isgreater than 1.5:1, preferably greater than 5:1 and more preferablygreater than 8:1;c) drawing in liquid medium, which takes place between the first tworoll towers of the pre-recuperator, while the yarn is submersed in thetank, wherein: a temperature between room temperature and 80° C. isadopted when water is used as a drawing medium in a liquid bath; and atemperature greater than 80° C. is adopted when the first solvent itselfis used as a drawing medium in a liquid bath, while a draw ratio greaterthan 8:1 is applied to the gel yarn;d) a residence time in the yarn accumulator of greater than 0.5 minute,preferably, a residence time of greater than 1 minute and morepreferably greater than 2 minutes, which will allow for a fraction ofstable volume to be transformed into free volume, and can also beretained in the second pre-recovery enclosure.

It is then clear that retention of the higher amount possible of thefirst solvent, ensured by the optional configuration of the proposedpre-recuperator, represents a great technical and economic advantageover the state of the art. However, recovering in an efficient mannerthe larger volume possible of the first solvent prior to feeding theextractors is not the only advantage described by the present invention.

To render the mineral oil based technology even more competitive thanthe decalin based technology, when all the aforementioned aspects aretaken into account, it is also interesting to develop concepts relatedto a greater efficiency of the extractors 50. Therefore, the presentinvention further discloses an extractor 50 with an advantageousconstruction feature, as will be discussed below.

FIG. 4 illustrates an extractor 50, in accordance with an optionalconfiguration of the present invention, comprising a rotating member,optionally illustrated as a rotating drum 52, that follows theconduction rules in rolls used in drawing godets and dual-type rolls,commonly used in the textile industry. The physical principle usedensures that one can wind the yarn in the same roll 52 (main roll)several times in such a way that they do not touch and/or entangle witheach other while being conducted. This is possible as an auxiliarymember, optionally in the form of an auxiliary roll 53 of smallerdiameter is used to separate the yarns by a distance that is a functionof the relative angle between the shafts of the two rolls 52,53.

In context of the present invention, the main roll 52 will behereinafter designated as drum 52. This designation is pertinent sincethe diameter thereof is larger than the diameter of the auxiliary roll.Such drum 52 has a rod crown 521 serving to carry the yarn while exposesthe filaments thereof to two streams of washing liquid 512,511. When theyarns are produced continuously and when no twist operation is applied,the yarn filaments accommodate under ribbon shaped surfaces. In otherwords, the yarn filaments are arranged almost perfectly in parallel toeach other. It causes the extraction liquid jets 511, 512 to reach thetwo larger faces of said ribbon, resulting in an effective contact.

Visually, when one yarn or a set of yarns is adjusted and conveyed overthe drum 52 a web is formed, which is subjected to the action of jets511, 512 on both sides. The relative angle between the drum axes 52 andthe auxiliary member 53, the distance between them and the diameterratio thereof define the spacing between the several yarns.

Using a structure with hollows, preferably rods 521, instead of a flatsurface is one of the advantageous aspects of the drum 52 of the presentinvention related to the high efficiency of the described extractor 50.With such a configuration, the drum 52 may receive jets 511, 512directed from both the internal and external faces. Thus, the yarn thatnaturally organizes itself in the form of a ribbon with filaments almostperfectly arranged side by side is subjected to an intense turbulentflow by the joint action of two jets arranged in opposite directions.

Using suitable liquid flow generating devices 511, 512, preferably jets,the extraction efficiency increases even more. Dispersing nozzles withjets of several geometric shapes can be used. There are commercialnozzles having a homogeneously intense jet along its geometric form,which is ideal to be adapted over the entire surface of the drum 52,both external and internal. Due to the geometric shape of the drum 52,square or rectangular jets are preferred.

The auxiliary member 53, in turn, has its axis attached to a mechanicalangle adjusting device, which can be adjusted even during operation incase the yarns wind in the drum 52. This adjustment is made by externalregulation, not requiring opening the equipment's door nor interruptingthe system operation.

For the purposes of the present invention, any device for changing theangle of the auxiliary roll can be used, provided that there is a propersealing between the regulation and the internal portion of theextractor.

Optionally, the jets nozzles are externally supported by a circularsupport 54 or by the extractor case 58, and is internally supported by afixed drum 55, which is a cylindrical structure that projects into theextractor. The drum can be moved by the movement of the yarns themselvesthat would then be conveyed by equipment before and after the extractorsor can be moved by an independent motor 57 via a drive shaft.

Optionally, the independent motor-driven drum 57 is preferred, whichprovides some advantages such as better titer control and thepossibility of applying drawing between extraction units when extractors50 in series are used.

In the extractor dynamics, the gel yarn rich in the first solvent entersthe first extractor 50 while the yarn rich in the second solvent exitsthe extractor.

FIG. 5 illustrates a representation of the perspective view of theoptional configuration of the drum of the present invention, where fiveyarns are fed into the extractor 50 spanning the entire area thereof.Variables as drum diameter 52, distance between the drum 52 shafts andthe auxiliary roll 53, number of turns of the yarn and tangential speedof the drum determine the contact time between the gel yarn and thewashing liquid.

The contact time or residence time is another critical parameter thatwill be discussed below. For a better use of the extractor 50, the mostnumber of turns as possible is given in the drum 52 area for each yarn.This is made possible by optimizing the angle ratio between the drum 52and the auxiliary roll 53.

In order to provide the greatest positioning stability of the yarn onthe drum and auxiliary roll surfaces, optionally one can use auxiliarypositioning devices. Optionally, comb-type spacers can be used in thepath of the yarn bundle located between the drum 52 and the auxiliaryroll 53. The comb spacing determines the number of turns of the yarn inthe drum and helps in stabilizing transportation, working together withthe auxiliary roll. The number of combs, the position and thepositioning angle thereof are irrelevant, but can be optimized for thefrequency of windings to be maximally minimized.

The yarn transport mechanism used in the present invention allows theextractor 50 not to lose efficiency with the increased speed caused bydrawing performed in steps prior to the extraction step. This ispossible because while the draw ratio is increased in the previoussteps, which increases the speed in the extraction unit, the yarnoccupancy width on the drum 50 reduces proportionately. In the contextof the present invention, occupancy width is defined by the width of thedrum occupied by each turn of the yarn. That is, the greater the drawratio applied to the yarn in any previous step, the higher the speed ofthe yarn in the extractor, but the lower its occupancy area by allowinga greater number of turns to be given for each wire. That is, thegreater number of turns compensates the increased speed. Therefore, thecontact time between the yarn and the second solvent applied by thewashing liquid delivery devices 511, 512 will be maintained almostconstant. Unlike other yarn extractors used in the spinning gel methodof the state of the art, the extractor described in the presentinvention allows for a great versatility of the method without therequirement to add extraction units to ensure complete removal of thefirst solvent in the output of the extraction unit.

Optionally, the extraction system is isolated from the externalenvironment by a protective wrap 58, or case, by an access port (notshown) and a mechanical seal mechanism at the entry and exit points ofthe yarns. Geometry of the case 58 can be optimized such that theinternal volume will be only that which is strictly necessary toaccommodate the drum 52 and the washing liquid delivery devices 511,512. Both the case 58 and the port are sealed so that no liquid or steamemanates out of the extractor 50 and are sized to withstand theoperating pressure.

A critical aspect of the oil based spinning gel method is that solventsused in the extraction usually have high vapor pressure. Use of thesesolvents enables drying of the yarn to be made at temperatures wellbelow the softening temperature of the xerogel yarn. While drying isfacilitated by the use of high vapor pressure liquids, the extractionstep becomes a point of high solvent evaporation rate. And if a goodinsulation system is not used, a large amount of the second solvent willbe lost at this step, which, in addition to the operational cost issues,prejudices health- and environmental-related aspects.

Therefore, complete isolation of the case 58 as well as the possibilityof pressurization is an important optional feature of the extractordevice 50 of the present invention, and can be achieved by using sealingdevices or mechanical seals at the entry and exit points of the yarn443. Any device that isolates the interior of the enclosure from theexternal environment can be used. However, in context of the presentinvention, Foulard devices especially designed for complete seal arepreferred.

FIG. 6 is a diagram containing an example of an optional configurationof valves and instruments used so that the extractor described by thepresent invention can operate using any volatile and flammable solventin a safe and sealed manner. FIG. 6a shows the extractor case containingall the yarn transporting and sealing mechanisms.

FIG. 6, in particular detail 6 a, illustrates an optional configurationof a sealing device for an extractor provided by the present inventionwherein the mechanical seal shown is formed by the yarn entry cavity,outlet cavity, rolls consisting of a metallic shaft, roll rubber andinternal sealing rubber. The roll rubber optionally has low stiffnessfor any damage to occur to the yarn. One can optimize the roll rubberpart using rubbers that are more resistant to friction in the endstogether with a soft rubber in the center where the yarn passes. Itreduces the maintenance cost of this type of device. The rubbercomprising the inner seal may be composed of high friction strengthrubber. All the elastomeric material used must withstand the continuousaction of liquids used as the first and second solvents.

Movement of the rolls should be ensured by a precise mechanism so thatthe tangential speed of the two rolls is equal to, or slightly smallerthan the yarn speed in the first extractor drum and equal to or slightlygreater than the drum speed of the last extractor. It can be done byusing an independent motor or by using the same mechanical system thatdrives the drum.

As already shown, Foulard-type devices are preferred in the presentinvention as they withstand high pressures and exhibit great sealing,preventing vapors to be released to the industrial environment.

In the lower portion of each extractor, a collecting vessel 56, alsodesignated extractor vessel, is optionally installed, which functions tocollect all the liquid projected by the washing liquid delivery devices511, 512, after contacting the yarns, to provide feedback to theinternal circulation system. To compose the internal circulationcircuit, a pump sucks the liquid from the vessel 56 and pressurizes afeed manifold of the internal 511 and external 512 nozzles through atube.

In order to control the washing temperature, a heat exchanger (notshown) is optionally used for removing or providing heat to (or heatingor cooling) the circulating fluid (second solvent) in relation to theextractor equilibrium temperature.

The circulation flow rate is another relevant aspect to the efficiencyof the extractor 50 of the present invention. Injection of clean solventis made by any liquid metering pump, provided that there is a good flowrate control between the reservoir and the interior of the extractor.Also, for a good utilization of clean solvent to ensure that the samecontacts the yarns, the internal circulation pump is preferablypositioned at a point below the extractor vessel.

In turn, disposal of spent solvent is done by any device consisting ofvalve and a level control. That is, the spent solvent disposal valveopens whenever a certain level is reached in the vessel. For definitionpurposes, in the context of the present invention, clean solvent is allliquid used as the second solvent with low or no content of the firstsolvent, whereas spent solvent is the liquid used as the second solventand having a higher concentration of the first solvent than theconcentration thereof in the so called clean solvent. Disposal point ofthe spent solvent is not critical. However, in order to prevent build-upor any dead spots, the disposal point is preferably located in a lowerportion extractor vessel 56.

A discharge valve is also optionally installed in the bottom of theextractor vessel 56, being activated each time the level sensor isactuated. Any level control device may be used.

Detail B of FIG. 6 presents a diagram of a skid containing a set ofvalves and instruments serving to, along with the inert gas supply skid(detail D), purge the extractor such that all oxygen from the air isfully expelled and to maintain the desired pressure for operation of theunit. The skid contains a reliable device for measuring the oxygencontent, so that an adequate intake of inert gas is used to ensureinertization of the interior of the extractor. The skid should, however,have a set of valves such that a high and low flow rate can be adjusted.High flow rate serves to purge the extractor, at the machine startup orevery time the port is opened. In turn, the low flow rate functions toenable small reliefs of pressure when the internal pressure of theextractor reaches a critical value.

The skid is adapted at the top of the extractor such that any solvent inliquid form enters the tubing. The skid outlet pipe can be connected toan exhaustion line or connected to the solvent recovery area. For thepurposes of reducing the solvent emanation rate to the environment, itis preferred to send the gases and vapors to the solvent recovery area.

Detail D of FIG. 6 shows a diagram of an inert gas supply skid that canbe used in the present invention and functions to feed inert gas to theextractor. The set of valves and instruments allows one to feed inertgas in high flow rate during the purge step, or in a low flow rate ofinert gas during operation in order to replenish any losses caused byleakage, keeping the internal pressure at a given constant target value.The high flow rate line acts at the time of purging, every time the portis opened or every time the oxygen content reaches a critical value forsafety of the equipment.

Additionally, a low flow rate meter can be used to monitor for possibleleaks in the extractor 50. Monitoring this flow rate allows forinterrupting the system operation for maintenance purposes, ensuringthat the environment is not contaminated by solvent vapors.

Detail F of FIG. 6 shows the internal circulation diagram, as describedabove, comprising the vessel, the internal circulation pump, the heatexchanger (not shown) and feed manifold of washing nozzles, togetherwith its valves and control instruments.

Detail E of FIG. 6 shows a diagram of the spent solvent disposal skid.The skid has a set of valves and control instruments that allow for thevolume of solvents contained inside the extractor to be rapidlyeliminated in case of emergency, as well as a set of valves andinstruments having the function to maintain the level of the circulationvessel constant.

Detail G of FIG. 6 shows the clean solvent supply line in the suction ofthe internal circulation pump, as described above.

In order to reduce consumption of clean extraction solvent, theextractor described in the present invention can optionally beassociated with others in a serial configuration. When the extractordescribed in the present invention is mounted in a serial configuration,the yarn fed into the first extractor passes to the other ones through aconducting channel adapted at the Foulard position. Foulard-type devicescan be used to fully isolate one unit from the other. However, in orderto prevent excessive deformation of the yarn, a conducting channel,having an inclined plane on its bottom, is preferred. The inclined planehas the function to cause any excess of spent solvent falling from theyarn to be always kept in the dirtiest (previous) unit.

Feed of clean solvent is preferably made in the last unit, where theyarn has the lowest content possible of the first solvent.

In the optional configuration in series, transfer of waste liquid can bedone via a dosing pump installed between the units, or simply by acascade-type overflow. Liquid flow between the cascade-type overflowunits takes place using drains joining the circulation vessels. In thesedrains, the liquid flows by gravity from one vessel to the other by adifference in height relative to the ground. In this configuration, thecleaner liquid moves by overflowing, always towards the dirtier unit, incountercurrent to the direction of the yarn, which moves from thedirtier to cleaner unit. The difference in height between the drainsensures that no liquid from the dirtier unit goes to the cleaner unit.In the context of the present invention, the cascade-type configurationis preferred. It reduces the equipment costs and simplifies the methodof fluid transportation.

In the optional serial configuration illustrated in detail E of FIG. 6,the disposal skid is installed on the first unit (richer in the firstsolvent), ensuring that the liquid inventory inside all the extractorsremains constant. To ensure that the inventory is quickly discharged incase of an emergency, high flow rate discharge valves can be installedin all units. In a normal operation situation, then, the clean solventfeed flow rate fed into the last unit is almost equal to the spentsolvent flow rate discharged in the first unit, provided there is noloss of solvent by evaporation.

The inert gas supply skid for purging and controlling pressure, asdescribed (detail D, FIG. 6) as well as the skid for purging andcontrolling the top pressure (detail B, FIG. 6) are equally connected toall units so as to ensure that oxygen is not at any dead spot of theserial units.

As will be discussed below, the use of extractors in series is intendedto decrease the consumption of clean solvent. At a balancing stage ofthe method, a concentration gradient of the first solvent will be formedbetween the first and the last extractors. The number of extractors usedwill then be the result of a cost/benefit ratio between the capitalexpenditure, added per each added unit, to the reduction of the cost ofsolvent separation operation in the solvent recovery unit.

There is also a possible decrease of investment in the solvent recoveryunit with the increased number of extractor units, by reducing thevolume of the tanks and distillation and purification columns. Thisreduction takes place because the mixture volume (first+second solvents)is reduced by increasing the number of extraction units, by reducing thevolume of the second solvent (the disposal solution of the first unitgets more concentrated in the second solvent as the number of serialunits increases). The number of extraction units, in series, is afunction of variables such as the maximum estimated speed after thepre-recuperator, the linear density of the yarn in the feed, the numberof yarns, the number of filaments per yarn, the occupancy width of theyarn in the drum and the efficiency to be considered at each step.

It is important to emphasize that when the first non-volatile solvent atnormal method conditions (dissolution temperature between 150° C. and310° C.) is a hydrocarbon, second solvents such as hydrocarbons,chlorinated hydrocarbons, chlorofluorocarbons and other organic solventssuch as diethyl ether and dioxane as well as a mixture/combinationthereof can be used. In context of the present invention, low boilingpoint hydrocarbons are preferred. Non organo-halogenated solvents withboiling points of less than 80° C., preferably less than 70° C. arepreferred. Organo-halogenated solvents have good dissolutionperformance, low boiling points and are not flammable.

Therefore, the method for the extraction of porous yarns of the presentinvention is based on the substitution of the first solvent with thesecond solvent, which takes place by the gradual dissolution of thefirst solvent by the second solvent in the extractor. In this context,the extraction system can be divided into two liquid phases. The firstliquid phase is the phase delimited by the surface of the yarnfilaments, i.e., the liquid phase contained inside the pores and on theouter surface of the yarn filaments. The second liquid phase is theliquid medium external to the yarn, i.e. the phase formed by liquidsurrounding the extractor. When a gel yarn segment contacts a certainvolume of extraction solvent there will be a gradual dissolution of thefirst solvent. Over time, the concentration of the first solvent in bothphases tends to be the same. For example, solvents such as n-hexane arefully miscible with mineral oil at any proportion. However, there is anissue of dissolution kinetics, since for the complete mixture to occur,the second solvent must permeate the porous structure, where there areinteractions with the polymer surface, making the method difficult.Generally, this dissolution kinetics is dependent upon factors such astemperature and the level of turbulence.

To describe the performance of a particular extractor, contactparameters between the two phases described above must be taken intoaccount. The science related to the extraction unit operation is broad,where many variables are involved. However, in the context of thepresent invention, aspects related to contact of the two phases will bediscussed. The extractor efficiency is therefore dependent on: (i) thecontact time between phases, (ii) the contact temperature and (iii) thecontact efficiency.

The contact time between the phases, or simply the residence time of theyarn inside the extractor, is dependent upon geometric factors as wellas the yarn speed. Geometric variables of the extractor define the pathtraveled by a yarn segment inside the extractor and which will be incontact with the liquid extraction medium. The perimeter of each turn isa function of the drum diameter, the auxiliary roll diameter and thedistance between the drum and the auxiliary drum shafts. In turn, thenumber of turns of each wire on the drum will be, in the presentcontext, the largest number possible. After defining the maximum widthavailable for each yarn, the number of turns is defined by the occupancywidth of the yarn on the drum and the minimum spacing for a lowprobability of entanglement during the extraction operation. Theoccupancy width is dependent on the number of yarn filaments, the yarntiter, the oil content present in the yarn, and so on.

FIG. 7 shows a conceptual diagram of the composition of the firstsolvent in the two phases involved with the contact time in theextractor. In such a diagram, one notes that the contact time is equalto zero, the liquid phase contained in the pores of the yarn iscompletely filled with the first solvent. At this moment, the firstsolvent composition, at this phase, is equal to 1. The phase formed bythe volume of extraction liquid (second solvent) inside extractor is inturn practically comprised by neat solvent and the first solventcomposition at this phase is equal to 0.

With the contact time, the composition of first solvent of thesurrounding phase begins to increase, whereas the composition thereof inthe yarn phase begins to reduce. If there is enough time for this totake place, the two phases will converge to same composition. In thecontext of the present invention, the second solvent is deemed to bedissolution solvent, whereas the first solvent will be treated as thesolute in the dissolution. The time at which the composition of firstsolvent (solute) is equal in both phases is deemed the critical contacttime (t_(c)*) and the composition of first solvent in the mixture isdesignated critical composition (φ*).

When the yarn contact time inside the extractor is less than thecritical time, the first solvent composition in both phases can bedescribed by the partition coefficient (P_(n)) and is given by equation1, where n represents the number of the extractor where analysis isbeing made. The partition coefficient is useful to define thecomposition of the first solvent, in the yarn phase, in each extractionstep and is obtained from the experimental curve described by the twocurves shown in the conceptual figure (FIG. 7). The partitioncoefficient tends to 1 with the contact time. The experimentaldetermination of the curves shown is important to define the operationalparameters of the extractors as well as the efficiency thereof. Contacttimes greater than t_(c)* are not necessary, since no reduction in thefirst solvent composition will take place in the yarn phase from thatpoint. In the context of the present invention, the yarn should remaininside each extraction unit for a time sufficient for the partitioncoefficient to reach a value greater than 0.5, preferably greater than0.8.

$\begin{matrix}{P_{n} = \frac{\varphi_{m}^{{circundant}\mspace{14mu} {fase}}}{\varphi_{n}^{{yarn}\mspace{14mu} {fase}}}} & {{Equation}\mspace{14mu} (1)}\end{matrix}$

The critical contact time, defined as the moment when the first solventcomposition reaches the same value in both liquid phases involved, canbe used as a parameter for measuring the extractor's efficiency. Thatis, the lower the critical time reached for a given operation condition,the more efficient the extraction method. For the extractor described bythe present invention, the critical contact time defined by t_(c)* ismainly influenced by the contact temperature and the contact efficiency.Naturally, the contact temperature follows the basic laws of organicsolvent dissolution and should be as high as possible. Where the firstsolvent is mineral oil and the second solvent is, for example, n-hexane,the contact temperature should be greater than 10° C., preferablygreater than 30° C., more preferably higher than 40° C. However, due toan excessive pressure inside the extractor, the temperature should beless than 60° C.

The other parameter that influences the critical time is the contactefficiency. In the context of the present invention, the contactefficiency is defined as the volumetric fraction of the total volume ofsurrounding liquid in the extractor, which actually comes into contactwith the yarn filaments from the nozzle jets.

The volumetric fraction that circulates inside the extractor withoutcontacting the yarn filaments should be as low as possible. To minimizethis, a suitable directing of the nozzles should be done. Usually, thenozzles manufacturer defines the distances and directing angles. Anotherparameter related to the contact efficiency is the force exerted by thejet on the yarns. The force of the jets, regulated by the individualflow rate of each nozzle, is the variable that can be manipulated in thecontrol of the force. The higher the force, the better the efficiency.However, the force will be limited by some damage or undesireddisplacement on the yarns on the drum.

The number of nozzles is another important parameter for efficiency. Thegreater number of nozzles, the greater the region of the drum that willbe subjected to the action of the jet force. One way to quantify this isby the percentage of the total area of the drum which will undergodirect action of the bundle from the nozzle. In the context of theinvention, the percentage of the total surface (inner and outer surfaceof the drum) must be greater than 50%, preferably greater than 80%.However, there is an economic factor that is related to the number ofnozzles for achieving this percentage. The greater the number ofnozzles, the greater the circulation flow rate and accordingly thesizing of the circulation pump. In the design of an industrial-sizedunit, it significantly affects the capital expenditure in the extractionunit and a cost-effectiveness calculation should be done for one toarrive at optimal machine settings.

Further, besides the direct action of the contact force of the jets onthe yarns, which results in an efficient level of turbulence thatreduces the mixing time, the internal circulation flow rate is also animportant parameter of solvent homogenization (first and secondsolvents). An internal circulation flow rate much greater than theextraction liquid feed flow rate is another important efficiencyparameter in the context of the invention (equation 2). In anequilibrium stage, the first solvent composition in the volume ofsurrounding liquid should be as homogeneous as possible in all places ofthe extractor where the liquid circulates. In this context, thecirculation flow rate has the same role as a stirring impeller in mixingvessel.

Q1>>Q2  Equation 2:

FIG. 7 further illustrates the diagram of the flow streams involved inthe extraction method. Each meter of yarn inserts in the extractor acertain volume of solvent. This stream is defined by “v” and isequivalent to the flow rate designated herein as “linear drag flowrate”, that is, the product of the yarn speed multiplied by the volumetransported by one meter of yarn. Flow rate Q₁ is the circulation flowrate whereas Q₂ is the feed flow rate of the second solvent. Since thesystem works at a constant level, Q₂ is also the drain flow rate,provided that the amount of solvent lost by evaporation is notsignificant. In general, the yarn enters rich in the first solvent tothe left and exits to the right rich in the second solvent. While theextraction solvent is fed on the opposite side to the yarn and exitsrich in the first solvent to the left. The contact time of the yarn withthe extraction fluid is given by the dimensions of the drum and theauxiliary drum, by the number of yarn turns in the drum and by the yarnspeed. For a suitable efficiency to be achieved, equation 2 must befollowed. It ensures that the concentrations of the internal phase ofthe pores tends to the concentration of external fluid.

Thus, in context of the present invention, the extractor disclosedherein optionally comprises at least one of:

a) a yarn transporting device comprising a main roll 52 and, optionally,an auxiliary roll 53, wherein, the main roll 52 comprises on its yarnconducting surface supports exposing both faces of the yarn web to theextraction liquid jets, and the auxiliary device 53, preferably anauxiliary roll that moves in the same tangential speed as the main roll,has an angle adjusting device such that one can regulate the spacingbetween the transported yarns preventing entanglement or to adjust theoptimal spacing for a good use of the occupancy width of the yarns onthe main roll;b) a yarn transporting mechanism where a large number of turns can beprovided, such that the residence time reduced by an increase in thespeed caused by a modification in the draw ratio applied to the yarn inprevious steps can be compensated;c) a closed pumping circuit of the extraction liquid, where a pumpconnected to a container mounted on the bottom of the extractor forcesthe extraction liquid to come into contact with the yarn web;d) a closed pumping circuit of the extraction liquid, where spray-typenozzles that project a jet in an homogeneous manner over the yarn webare used, wherein said jet has a suitable geometry such that most of thesurrounding liquid contacts the web yarns;e) a closed pumping circuit of the extraction liquid, having control ofthe circulation pump motor rotation, such that the circulation flow ratecan be either increased or reduced to ensure that the force of thespray-type nozzles on the web yarns is suitable;f) a closed pumping circuit of the extraction liquid, where a suitablenumber of nozzles 511, 512 is used such that the majority of theinternal and external surface of the main roll is subjected to theaction of the internal circulation jets of extraction liquid;g) a closed pumping circuit of the extraction liquid, where a heatexchanger is used to transfer or remove heat from the surroundingliquid;h) an insulation case 58 from the external environment, where a skid ofvalves and instruments is used to purge its inner atmosphere with aninert gas, whenever a flammable liquid is used as the second solvent inthe extraction liquid, where a reliable instrument measures and monitorsthe oxygen concentration, so that the explosiveness of the internalatmosphere is null;i) an insulation case from the external environment, where a skid ofvalves and instruments is used for a positive gauge pressure be set byusing a constant feed of inert gas, wherein the pressure control can beadjusted so that the pressure is slightly above the vapor pressure ofthe extraction liquids, ensuring that the second solvent remains in theliquid state during the extraction operation;j) an insulation case from the external environment containing a set ofmechanical seal 59 at the inlet and outlet positions of the yarn in theextractor 50, such that a good seal under the yarn is provided withoutany damages caused by some kind of deformation occurring to the same;l) an insulation case from the external environment containing a sealedport that opens and closes in a practical and safe manner exposing theyarns under the transportation rolls whenever an intervention isrequired;m) a feed circuit of the second clean solvent that functionsautomatically with an extraction liquid disposal valve, rich in thefirst solvent, with the aid of a drain, so as to ensure that the volumeof extraction liquid inside the extractor is almost always the same;n) a circuit characterized by having a clean solvent feed dosing pump,where the injection point is mounted on the unit that is richer in thesecond solvent, wherein the circuit is further characterized bycontaining a an extraction liquid disposal drain mounted on the unitthat is richer in the first solvent.

Furthermore, in context of the present invention, when a set ofextractors is optionally adopted for the extractor to comprise multiplestages, the set of extractors comprises the following features:

a) it has a number of extraction stages where n units, as describedabove, are mounted in series, and where such a number of extractionstages is greater than one, preferably greater than three;b) it has a set of n extraction stages, where the yarn rich in the firstsolvent is fed to the first extraction stage, while the yarn rich in thesecond solvent exits the nth extraction stage, wherein an extractionliquid rich in the second solvent is fed in the nth stage, while theextraction liquid rich in the first solvent is discarded in the firststage, such that when a set of extraction units is used, the extractionliquid stream moves, optionally by a cascade-type overflow, in acontinuous stream that goes from the nth extractor to the firstextractor, wherein such overflow takes place in pipes connecting theinternal and circulation vessels of the extractors;c) it has a contact time in each stage given by the dimensions of thetransportation mechanism described above, such that there is ahomogenization of the yarn and surrounding medium phases, such that apartitioning coefficient greater than 0.5, preferably greater than 0.8is reached in each of the units;d) it has an optimized contact efficiency in each stage to achieve thelower critical time (tc*) for each unit, such that:

-   -   the internal circulation flow rate (Q1) is greater than the feed        flow rate (Q2) of the second solvent;    -   the number of jet nozzles of the spray type is used such that        the area of action of the jets covers at least 50% of the total        area (outer surface+inner surface of the web), preferably        greater than 80% of the total area of the yarn web;        e) it has, by means of the heat exchanger, a regulated        temperature control in all extraction units, such that the        temperature is determined as a function of the boiling point of        the liquid used as the second solvent, and should be as high as        possible, such that the maximum working pressure of the        extractors is not exceeded.

Thus, in accordance with the optional configuration of the presentinvention described so far when the yarn exits the extractors 50, almostthe entire the volume of the first solvent is substituted with thesecond solvent. Subsequently, the gel yarn containing the less volatilesolvent (second solvent) is then subjected to a drying process at a lowtemperature in order not to damage the microstructure thereof.

FIG. 1 further illustrates an optional configuration of a drying device6, or dryer, which can be used according to the present invention. Anyyarn, ribbon and/or fabric drying devices known in the state of the artcan be used for the purposes of the present invention. However, in orderto avoid variation in the titer or linear density of the yarn duringdrying, biased zig-zag conveyors in all the conveyor rollers and aprecise stress control, wherein the conveyor rollers 61 can also beheated. Further, any homogenous heat source can be used, but heatedinert gas forced circulation is optionally adopted.

Optionally, the drying device further comprises at least one dry gasinlet aperture and at least one wet gas outlet aperture, such that a gasis circulated in a closed-loop between the dryer 6 and the recoveryunits 5 of the second solvent.

When the yarn exits the drying unit, with practically no residue of thesecond solvent, it is designated xerogel yarn. Xerogel is a term used insol-gel chemistry to describe a gelled structure that lost the liquidphase (dry gel).

The xerogel yarn is then continuously fed to at least one cold drawingroll tower 7, optionally two, as illustrated in FIG. 1. For the samereason as discussed for gel yarn drawing, it is economically interestingthat the drawing portion can be cold, especially due to the orientationof the amorphous phase, provided that the limit of damage to thecrystalline structure (that has no cold motility) is respected. However,this step is optional.

The pre-drawn xerogel yarn is then subjected to a hot draw process in ahot drawing device 8. It should be noted that hot drawing can be made ina single stage or multiple stages. Thus, the schematic illustration ofcomponents set out in FIG. 1 is intended to provide understanding on themethod. Other types of ovens, rolls and drawing godets and types ofovens present in the state of the art can be used in the hot drawing ofthe method described in the present invention.

Finally, the yarn is wound on a winding unit 90. Between the end of thehot drawing and the beginning of winding, the yarn may receive anyfinishing used in the state of the art to provide the yarn with someimprovement in its properties and processability in the finalapplication. Any winding device disclosed in the state of the art canalso be used to wind the yarn. Since the method is continuous, there isno limit to the weight of the bobbin in question.

For the purposes of reducing costs related to a drawing machine or togain mechanical properties, the yarn obtained by the method described inthe present invention can be drawn somewhere else where a drawingmachine having suitable dimensions and length can be used. Where thistype of configuration is used, the method of the present invention willbe characterized as semi-continuous.

The figures and steps described herein are assumed in such a way for abetter understanding of the ideas contained in the document, but canvary depending on the understanding of a skilled person.

Therefore, in summary, the present invention provides the following:

-   -   a system for dosing a polymer mixture with a first solvent in an        extruder (26) comprising at least two inertization devices        (21,22,23) comprising means for introducing an inertization gas        flow, and that the at least two inertization devices (21,22,23)        feed the extruder (26) with the inertized mixture, further        comprising a feeding control device adapted to control the        mixture level above the screw (261) of said extruder (26), such        that rotation is sufficient not to segregate phases in the        mixture;    -   a dosing method of a mixture with a first solvent in an extruder        (26) comprising the steps of inertizing the mixture with an        inertization gas flow in an inertization device (21,22,23) and        feeding the extruder (26) with the inertized mixture,        the method further comprising controlling the mixture level        above the extruder screw.    -   a solvent extraction device of at least one polymeric yarn        comprising a first solvent comprising: a rotating member (52)        comprising a structure having hollows (521) in which the at        least one polymeric yarn is externally wound at least one once;        at least two extraction liquid delivery devices (511, 512),        wherein at least one of the at least two washing liquid delivery        devices (511, 512) is designed to deliver the washing liquid to        the at least one polymeric yarn externally to the rotating        member (52), and at least one of the at least two washing liquid        delivery devices (511, 512) is designed para deliver the washing        liquid in at least one polymeric yarn internally to the rotating        member (52).    -   a method for mechanical pre-recovery of at least one liquid in        at least one polymeric yarn, wherein the at least one liquid        comprises at least one of a solvent and water, comprising the        steps of: receiving a polymeric yarn from a quenching bath (30);        and mechanically retaining at least one liquid of the polymeric        yarn surface in a first pre-recovery enclosure (42).    -   a system for mechanical pre-recovery of at least one liquid in        at least one polymeric yarn, wherein the at least one liquid        comprises at least one of a solvent and water, comprising means        for receiving a polymeric yarn from a quenching bath (30); and        means for mechanically retaining at least one liquid of the        polymeric yarn surface.    -   a method for the manufacture of at least one polymeric yarn        comprising the steps of: mixing a polymer with a first solvent        yielding a mixture; homogenizing the mixture; rendering the        mixture inert; dipping the mixture into a quenching bath (30),        wherein an air gap is maintained before the mixture reaches the        quenching bath (30) liquid surface forming at least one        polymeric yarn; drawing the at least one polymeric yarn at least        once; washing the polymeric yarn with a second solvent that is        more volatile than the first solvent; heating the at least one        polymeric yarn; drawing at room temperature the at least one        polymeric yarn at least once; and heat drawing the at least one        polymeric yarn at least once.    -   a system for the manufacture of at least one polymeric yarn        comprising: means for mixing a polymer with a first solvent        yielding a mixture; means for homogenizing the mixture; means        for rendering the mixture inert; means for dipping the mixture        into a quenching bath (30), wherein an air gap is maintained        before the mixture reaches the quenching bath (30) liquid        surface forming at least one polymeric yarn; means for drawing        the at least one polymeric yarn at least once; means for washing        the at least one polymeric yarn with a second solvent that is        more volatile than the first solvent; means for heating or        cooling the at least one polymeric yarn; means for drawing at        room temperature the at least one polymeric yarn at least once;        and means for heat drawing the at least one polymeric yarn at        least once.

Next, comparisons of the methods, systems and devices of the presentinvention and those known from the state of the art will be shown.Comparisons between the yarns produced by these processes will also bedisclosed.

Example 1: Determining the Pre-Recovery Index by a Batch Method

A jacketed, stainless steel vessel, which contains a jet mixingcirculation system, wherein a pump mounted to the lower part causesforced circulation of the suspension from the bottom to the top, wasloaded with 7 kg of a suspension containing 8% Utec 3041 (a ultra-highmolecular weight polyethylene manufactured by Braskem S.A.) in whitemineral oil (Emca Plus 350 Oil, manufactured by Oxiteno). In order toreduce degradation, 500 ppm Irganox 168 and 500 ppm Irganox 1010 wereadded, based on the total weight of the mixture. The vessel was closedby a lid containing a stirring rod with five vanes having an impellerangle of 45°, arranged 90° with respect to each other. The set of vanesstirs the entire suspension column. A rotation of 350 rpm was set, whilethe jet mixing pump was regulated for the entire initial inventory to berenovated in approximately 1 minute. A nitrogen stream was adjusted onthe bottom of the vessel such that the oxygen content, as measured by asensor mounted to the bottom of the vessel, achieves values of less than0.1 ppm in 40 minutes. After this time, the suspension was dosed to a 25mm twin screw Haake extruder. Dosing was made by means of a vesselcontaining a level sensor installed in the feeding zone of the extruder.Level control was regulated such that the level of dosed suspension wasroughly 10 mm above the screw. The dosage system is automated such thata low level signal is given to a gasket type valve present on the bottomof the suspension vessel, causing the same to open until a new signal offull level is sent by the extruder feeding vessel. This system ensuresthat only a sufficient amount of suspension is dosed to the extruder,preventing the existence of liquid columns with low level of agitation.A small column of suspension above the screw will be subjected to theagitation action of the screw itself. The temperature of the feed zonewas maintained below 60° C. while dissolution was carried out at atemperature of 210° C. The spinning die containing a spinneret with 15filaments of 0.5 mm in diameter was maintained at 190° C. The flow rateof the spinning pump was adjusted so as to achieve a mass flow rate of0.6 g/min for each capillary. The filaments bundle passed through a 10mm air gap and a water (quenching) bath at a temperature of 10° C. Theyarn was then pulled by a spinning godet at a speed of 4.2 m/min andthen wound using a Barmag winding machine in a plastic cartridge ofknown weight. A bobbin containing 1 hour spinning was collected and leftto rest under a support such that the axis of the cartridge is at 90°with regard to the bench surface. Therefore, the oil exuded from theyarn can drain to a tray within a period of 48 hours. After this period,the bobbin was weighted. Three yarn segments were removed in differentlayers of the bobbin for analyzing the oil content by a Soxhletextractor. Soxhlet extraction was carried out in accordance with RuleASTM D 2257 using n-hexane as the extraction agent. In order to providea comparative method, determination of the oil content by mass balancewas also used. There was a suspicion that mineral oil would migrate tothe surface of the bobbin over time, causing a concentration gradient,which could result in error. The total volume of mineral oil in thebobbin in one hour spinning can be calculated by the mass flow rate ofthe spinning pump, knowing that it contained 8% polymer. Based on theweight after 48 hours, the weight amount of pre-recovered oil could bedetermined. Based on this data, the pre-recovery index was thendetermined. As discussed above, the pre-recovery index is described bythe percent mass or volume ratio of solvent transported by a certainlength of the yarn that exits the pre-recuperator and the yarn enteringthe pre-recuperator. In the instant example, the pre-recuperator isdefined as the support where the bobbin rests for a certain period oftime, while the solvent is retained by the action of gravity (batchmethod). Then, after 48 hours of pre-recovery, a result of thepre-recovery index of 34% was obtained by Soxhlet, while a pre-recoveryindex of 24% was obtained by mass balance. These values will serve ascomparative values with data obtained by pre-recovery in a continuousmethod. The procedure described herein was performed in accordance withU.S. Pat. No. 8,003,027B2, where a mineral oil-based method isdescribed.

Example 2: Determining the Pre-Recovery Index by the Continuous MethodDescribed in the Invention, without Using Drawing in a Liquid Bath andOnly Using a Pre-Recovery Enclosure

Another experiment was carried out using the same procedure as describedin Comparative Example 1, but the yarn pulled by the spinning godet wasfed to the feeding rolls of a drawing machine in liquid medium, whichhas a tank having 1.2 m in length, containing water at a temperature of80° C. At the other end of the tank, a set of three rolls pushed theyarn fed to the first pre-recovery chamber. The draw ratio between thesteps was 1.02 with the exception of the drawing in the tank, which wasadjusted to 1.1. The first pre-recovery chamber contains a set of sevenmotorized rolls, where each roll has a compressed air flow generatingdevice of the air blade type from Spraying System, with the air flowpositioned in the opposite direction to the motion of the yarn and at atangent position to the roll. Each roll has a rubber scraper to removethe amount of oil adhered to the roll surface. The distance of the airblade generating device to the roll surface was set to 35 mm. The airpressure in the feed manifold of the air blade generating devices wasset to 5 bar. The Barmag winding machine was positioned after the firstpre-recovery chamber to collect the yarn, in the same manner as theprevious experiment. Bobbin samples were collected at each 30 minutesfor assessing the oil content, by both Soxhlet and mass balance. Theaverage pre-recovery index, as measured by Soxhlet, was 31%. While theaverage pre-recovery index, as measured by mass balance, was 23%.

Example 3: Determining the Pre-Recovery Index by the Continuous MethodDescribed in the Invention Using Drawing in Liquid Bath and Using aSingle Pre-Recovery Enclosure

The same experiment carried out in comparative Example 1 was performed,but using higher stretches in the drawing machine in liquid medium. Tothe remaining steps, drawing was maintained with a low draw ratio of1.02. Yarn samples were collected at each 30 minutes to determine theaverage index for each condition. To this experiment, only a Soxhletanalysis was used to determine the oil content. Results obtained to theexperiments using draw ratios greater than 1.1, carried out in thedrawing machine in liquid medium are shown in the Table I. Forcomparison purposes, the result obtained from the above examples wereincluded.

TABLE I Experiment Name Draw Rate Pre-recovery Index (%) Bath 48 hs — 34Continuous D.R. 1.1:1 1.1 31 Continuous D.R. 2:1 2.0 14 Continuous D.R.3:1 3.0 19 Continuous D.R. 5:1 5.0 34

Example 4: Determining the Pre-Recovery Index by the Batch Method UsingDrawing in Liquid Bath and Using a Single Pre-Recovery Enclosure

Bobbin collection samples at 1 hour under the same conditions aspresented in Example 3 were left under the support on trays for 48 hoursin the same manner as described in Comparative Example 1. The object ofthis Experiment was to determine the free oil fraction that cannot beretained or pre-recovered by the first pre-recovery chamber, by acontinuous method, in the previous Experiment. However, to thisExperiment, assessment of the oil content was made by mass balance.Results are set forth in Table II. Again, for comparative purposes, theresults of the indices determined in comparative examples 1 and 2 wereadded to the table.

TABLE II Experiment Name Draw Rate Pre-recovery Index (%) Bath 48 hs —24 Continuous D.R. 1.1:1 1.1 23 Continuous D.R. 2:1 2.0 27 ContinuousD.R. 3:1 3.0 30 Continuous D.R. 5:1 5.0 45

Example 5: Determining the Pre-Recovery Index by the Continuous MethodDescribed in the Invention Using Drawing in Liquid Bath and Using TwoPre-Recovery Enclosures

The present experiment was carried out under the same conditions asExample 3 but a second pre-recovery enclosure was used. The secondpre-recovery enclosure was built just like the first pre-recoveryenclosure, which was described in Comparative Example 2. To allow for alow exudation time to be given to the yarn, such that a stable oilfraction was transformed into free oil fraction, on the yarn surface, adistance of 4 meters was used between the two pre-recovery enclosures.Speeds of the two pre-recovery enclosures were adjusted such that a drawratio of 1.2 was applied between them in order to maintain the adhesivestrength of the inner rolls of both enclosures. For comparativepurposes, new bobbins were generated under the same conditions ascomparative examples 1 and 2. Barmag winding machine was then installedafter the second pre-recovery enclosure. The oil content in the sampleswas determined by mass balance. Results are set forth in Table III.

TABLE III Experiment Name Draw Rate Pre-recovery Index (%) Bath 48 hs —20 Continuous D.R. 1.1:1 1.1 24 Continuous D.R. 2:1 2.0 27 ContinuousD.R. 3:1 3.0 27 Continuous D.R. 5:1 5.0 38

Example 6: Determining the Influence of the Residence Time, Enabled byUsing the Accumulator, on the Pre-Recovery Index by the ContinuousMethod Described in the Invention

To determine the impact of the residence time between the twopre-recovery enclosures, two pulley bars were installed such that theyarn could increase its path between the enclosures. Due to the frictionadded per each pulley, the number of “zig-zag” turns was limited tofive. Therefore, the path between the two pre-recovery enclosuresincreased from 4 m to about 20 m. A greater number of turns could not bemade as the yarn started to fall from the latter roll of the firstpre-recovery chamber. Most likely it was due to the friction of the setof pulleys, which reinforces the use of motorized roll towers on theaccumulator. For this experiment, only larger draw ratios of 2.0 wereapplied. The experiment conditions were the same as applied to theexperiment described in Example 5. Data is set forth in Table IV.

TABLE IV Experiment Name Draw Rate Pre-recovery Index (%) ContinuousD.R. 3:1 2.0 43 Continuous D.R. 5:1 3.0 51 Continuous D.R. 7:1 5.0 61

To better observe the influence of the residence time on thepre-recovery index, data of the draw ratio condition applied to the yarnin the drawing machine in liquid bath of 3.0 was used. The residencetime was calculated as a function of the speed applied to the firstpre-recovery chamber and the path of the yarn in the accumulator. Forcomparative purposes, results of the above experiments for a draw ratiocondition of 3.0 were consolidated and shown in Table V.

TABLE V Experiment Residence Time (min.) Pre-recovery Index (%) Ex. 30.00 19 Ex. 5 0.22 27 Ex. 6 1.12 43

Example 7: Assessment of the Product Produced by the Continuous MethodDescribed by the Invention, Until the Pre-Recovery Step

For the purposes of assessing the impact of using the pre-recoveryoperation on the mechanical properties of the yarn, a series of bobbinscontaining a 1-hour spin were collected under the conditions describedin Example 6. For reference purposes, a bobbin collected under the sameconditions as described in Comparative Example 1, which has notsubjected to any equipment of the pre-recovery unit, was used. Themechanical properties were determined in accordance with ISO 2062 usingan initial length of 250 mm and a displacement speed of the crossbar of250 mm/min. An Instron pneumatic grip for textile specimens was used.Washing the bobbins with n-hexane, as well as the draw procedure, werecarried out in accordance with patent document U.S. Pat. No.8,003,027B2. Samples with draw ratios greater than 5.0 lack a goodperformance in the batch type extractor described in the cited patentdocument. From this draw ratio on, the yarns began to become too stiff,with yarns being wound in a too compact manner for n-hexane to be ableto percolate in the yarn layer of the bobbin. To these samples, it wasnoted an evident preferred path between the bobbin yarns in the batchtype extractor. As is known in the state of the art, mechanicalproperties get worse with the increase in the content of the firstsolvent in the xerogel yarn.

TABLE VI Experiment Name Draw Rate Tenacity (cN/dtex) Bath Process — 38Continuous D.R. 1.1:1 1.1 38 Continuous D.R. 2:1 2.0 36 Continuous D.R.3:1 3.0 38 Continuous D.R. 5:1 5.0 34

Example 8: Performance Assessment of the Extractors in the ContinuousMethod Described by the Invention

The same spinning formulation and condition as described in ComparativeExample 1 was applied to assess the extraction unit. A spinneretcontaining 15 capillaries was used. The flow rate of the spinning pumpwas adjusted so as to achieve a mass flow rate of 0.45 g/min for eachcapillary. The filaments bundle passed through a 10 mm air gap and awater (quenching) bath at a temperature of 10° C. The yarn was thenpulled by a spinning godet at a speed of 3.17 m/min and then fed to thepre-recovery unit. A small draw of 1.02 was applied in all theintermediate steps of the pre-recovery unit, with the exception of thedraw in liquid medium and in the Accumulator, where a draw ratio of 1.2was applied to the gel yarn. A continuous extractor containing fourextraction units was used to wash the gel yarn. A guide yarn was used toprepare the extractor to receive the gel yarn thus produced. Such guideyarn was passed through the Feed Foulard of Extraction Unit 1 and wasthen wound onto four Rotary Drums of the four units. In each drum, atotal of 14 turns were made. The drums are 600 mm in diameter and havean auxiliary roll of 60 mm. The distance between axes is of 600 mm.After passing the guide yarn, doors were closed, the units wereinertized with nitrogen until the oxymeter showed an oxygen content ofless than 0.1% (v/v). At this moment, the feed pump started loading theunits with clean n-hexane. After loading, the machine was pressurizedwith nitrogen up to a work pressure of 0.4 bar and this condition wasmaintained throughout the test. Circulation pumps of units 1, 2, 3 and 4were added and the Drums started pulling the gel yarn with the aid ofthe guide yarn. The contact time in each unit was of about 4 minutes atthe test speed. Feed rate was maintained at 12 L/h. The gel yarn at theoutlet of the extractors was fed to a yarn dryer from Mathis. The dryingtemperature was adjusted to 80° C. and the draw ratio between extractorsand the dryer was adjusted to 1.02. The Barmag winding device wasmounted on the outlet of the dryer to collect the xerogel yarn. Xerogelyarn samples were collected for assessing the residual oil by Soxhlet.The oil content in the circulation liquid was determined by an index ofrefraction using an calibration curve of oil in n-hexane. For increasingthe accuracy of the method, three calibration curves were made in threeranges of oil in n-hexane content. The results are shown in Table VII.

TABLE VII Values/ Values/ Values/ Values/ Extractor Extractor ExtractorExtractor 1 2 3 4 Input Yarn Speed (m/min.) 14.5 14.8 15.1 15.4 ContactTime (min.) 4 4 4 4 Oil-In-Yarn Inlet 90 * * * (wt %) Titre Yarn Inlet3720 * * * (dtex) Solvent Flow Rate 12.0 12.0 12.0 12.0 (L/h) Partition~1 ~1 ~1 ~1 coefficient (—) Extraction 35 35 35 35 Temperature (° C.)Output Recirculation Phase 5.1 0.3 0.04 <0.01 Oil-In-Solvent (wt %)Residual Oil-In- * * * 0.06 xerogel Yarn Outlet (wt %) *It wasn'tdetermined

Example 9: Assessing the Performance of the Extractors in the ContinuousMethod Described by the Invention Using a Single Extraction Unit

The present experiment was carried out as described in Example 8, but aspinneret of 34 filaments of 0.5 mm diameter was used. Only thecirculation pump of the extraction unit 1 was turned on. Results are setforth in Table IX. The results are shown in Table VIII.

TABLE VIII Values/Extractor 1 Input Yarn Speed (m/min.) 14.5 ContactTime (min.) 4 Oil-In-Yarn Inlet (wt %) 90 Titre Yarn Inlet (dtex) 8,434Solvent Flow Rate (L/h) 12.0 Partition coefficient (—) ~1 ExtractionTemperature (° C.) 35 Output Recirculation Phase 4.8 Oil-In-Solvent (wt%) Residual Oil-In-xerogel Yarn 22.8 Outlet (wt %)

Example 10: Assessing the Performance of the Extractors in theContinuous Method Described by the Invention Using Two Extraction Units

The same experiment was made as described in Example 9, but thecirculation pump of extraction unit 2 was also turned on. That is, thebehavior in extraction with two units was studied. Results are set forthin Table IX.

TABLE IX Values/ Values/ Extractor 1 Extractor 2 Input Yarn Speed(m/min.) 14.5 14.8 Contact Time (min.) 4 4 Oil-In-Yarn Inlet (wt %) 90 *Titre Yarn Inlet (dtex) 8,434 * Solvent Flow Rate (L/h) 12.0 12.0Partition coefficient (—) ~1 ~1 Extraction Temperature (° C.) 35 35Output Recirculation Phase Oil-In- 4.8 0.39 Solvent (wt %) ResidualOil-In-xerogel Yarn * 1.6 Outlet (wt %) *It wasn't determined

Example 11: Assessing the Performance of the Extractors in theContinuous Method Described by the Invention Using Three ExtractionUnits

The present Experiment was carried out as described in Example 9, butthe circulation pump in extraction units 2 and 3 were also turned on.That is, the behavior in extraction with three units was studied.Results are set forth in Table X.

TABLE X Values/ Values/ Values/ Extractor Extractor Extractor 1 2 3Input Yarn Speed (m/min.) 14.5 14.8 15.1 Contact Time (min) 4 4 4Oil-In-Yarn Inlet (wt %) 90 * * Titre Yarn Inlet (dtex) 8,434 * *Solvent Flow Rate (L/h) 12.0 12.0 12.0 Partition coefficient ~1 ~1 ~1(—) Extraction Temperature 35 35 35 (° C.) Output Recirculation Phase4.8 0.39 0.08 Oil-In-Solvent (wt %) Residual Oil-In-xerogel * * 0.24Yarn Outlet (wt %) *It wasn't determined

Example 12: Assessing the Performance of the Extractors in theContinuous Method Described by the Invention Using Four Extraction Units

To determine the index of clean n-hexane consumption to produce 1 kg ofxerogel yarn, a bobbin containing 90 filaments of gel yarn wascontinually fed into the extraction unit. The Experiment was carried outby changing the feed flow rate of clean solvent in the fourth unit, suchthat it was possible to measure the residual oil content in the xerogelyarn as a function of the flow rate, awaiting for the stabilization timeof the method. Data to the xerogel sample containing about 4% oil is setforth in Table XI.

TABLE XI Values/ Values/ Values/ Values/ Extractor Extractor ExtractorExtractor 1 2 3 4 Input Yarn Speed (m/min.) 14.5 14.8 15.1 15.4 ContactTime (min.) 4 4 4 4 Oil-In-Yarn Inlet 86 * * * (wt %) Titre Yarn Inlet57,410 * * * (dtex) Solvent Flow Rate 15.0 15.0 15.0 15.0 (L/h)Partition ~1 ~1 ~1 ~1 coefficient (—) Extraction 35 35 35 35 Temperature(° C.) Output Recirculation Phase 31.8 9.96 2.96 0.72 Oil-In-Solvent (wt%) Residual Oil-In- * * * 4.3 xerogel Yarn Outlet (wt %) Kg Solvent/Kg14.9 xerogel Yarn (—) *It wasn't determined

Example 13: Assessment of the Product Produced by the Continuous MethodDescribed by the Invention, where all the Steps are Used

A xerogel yarn was produced under the same conditions as described inexample 8. However, it was fed to a drawing machine comprising twotowers containing five rolls, wherein a draw ratio of 1.2 at roomtemperature was applied. Thereafter, the yarn was heat drawn using aRetech drawing machine. A draw ratio of 6,4 was applied at thetemperature of 135° C. to continually produce the POY yarn (Pre OrientedYarn). A bobbin of POY yarn was then fed to a FET drawing machine, wherethe yarn was drawn in two steps between the temperatures of 145° C. and150° C. A total draw ratio of 3.6 was applied to the yarn to obtain afinal yarn. The mechanical properties were obtained in accordance withISO 2062 using an initial length of 250 mm and a displacement speed ofthe crossbar of 250 mm/min. To determine the elastic modulus, avolumetric density of 970 kg/m3 was considered while calculating thecross section area of the filaments. An Instron pneumatic grip fortextile specimens was used (Tenacity=38 cN/dtex, Tensile Modulus=132GPa).

What is claimed is:
 1. A method of mechanical pre-recovery of at leastone liquid in at least one polymeric yarn, wherein the at least oneliquid comprises at least one of a solvent and water, comprising thesteps of: receiving a polymeric yarn from a quenching bath; andmechanically retaining at least one liquid of the polymeric yarn surfacein a first pre-recovery enclosure.
 2. The pre-recovery method of claim1, further comprising drawing the at least one polymeric yarn in adrawing tank comprising a liquid medium, wherein the liquid medium isheated prior to the step of mechanically retaining at least one liquidof the polymeric yarn surface; accumulating the at least one yarn inaccumulator rolls; and and mechanically retaining at least one liquid ofthe polymeric yarn surface in a second pre-recovery enclosure.
 3. Thepre-recovery method; of claim 1, wherein the step of mechanicallyretaining at least one liquid of the polymeric yarn surface comprises atleast one of generating an air flow against the surface of the at leastone gel yarn, and tangentially scraping the liquid from the accumulatorrolls.
 4. A system of mechanical pre-recovery of at least one liquid inat least one polymeric yarn, wherein the at least one liquid comprisesat least one of a solvent and water, comprising: means for receiving apolymeric yarn from a quenching bath; and means for mechanicallyretaining at least one liquid of the polymeric yarn surface.
 5. Thepre-recovery system of claim 4, further comprising means for drawing, ina drawing device, the at least one polymeric yarn in a drawing tankcomprising a liquid medium, wherein the liquid medium is heated; meansfor accumulating, in an accumulator device, the at least one yarn inaccumulator rolls; and means for mechanically retaining at least oneliquid from the surface of the at least one polymeric yarn in a secondpre-recovery enclosure.
 6. The pre-recovery system of claim 4, furthercomprising means for mechanically retaining at least one liquid of thepolymeric yarn surface comprising at least one of: at least one air flowgenerator against the surface of the at least one gel yarn; and at leastone scraper device designed to tangentially scrape the liquid from theaccumulator rolls.
 7. The pre-recovery system of claim 4, furthercomprising a feed roll tower device before the drawing device,comprising at least one roll and, positioned below them, a liquidcollection device.
 8. The pre-recovery system of claim 4, furthercomprising a second pre-recovery enclosure after the yarn accumulatordevice.
 9. The pre-recovery system of claim 4, wherein the pre-recoveryenclosure comprises an insulating housing designed to absorb noise anddesigned to retain liquid particles.